KR20000052120A - Method for prducing activated carvon using oxidizing power of ferric sulfate s - Google Patents
Method for prducing activated carvon using oxidizing power of ferric sulfate s Download PDFInfo
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- KR20000052120A KR20000052120A KR1019990002992A KR19990002992A KR20000052120A KR 20000052120 A KR20000052120 A KR 20000052120A KR 1019990002992 A KR1019990002992 A KR 1019990002992A KR 19990002992 A KR19990002992 A KR 19990002992A KR 20000052120 A KR20000052120 A KR 20000052120A
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- ferric sulfate
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
Abstract
Description
본 발명은 광유 특히 방카C유와 같은 중질유에 황산제2철을 혼합하고 300℃~500℃로 가열하여 제조되는 활성탄소의 제조방법에 관한 것이다.The present invention relates to a process for producing activated carbon prepared by mixing ferric sulfate in mineral oil, in particular heavy oil such as banca C oil and heating to 300 ℃ ~ 500 ℃.
활성탄소는 순수한 탄소(C)로된 미세입자로서 식품정제, 의약품정제, 상하수정제, 유독성가스의 제거 및 공해방지 시설물에 광범위하게 사용되고 있는 것으로 우리나라에는 연간3만톤정도 사용되고 있으며 대부분 중국, 일본, 미국에서 수입하여 사용하는 실정이다.Activated carbon is a fine particle made of pure carbon (C), which is widely used in food refining, pharmaceutical refining, water and sewage refining, and toxic gas removal and pollution prevention facilities. Imported from and used.
종래의 활성탄소 제조방법은 야자껍질을 비롯한 과일껍질이나 곡물류의 폐기물 톱밥등을 원료로하여 탄화시키고 물을 가하는 수증기 부활방법의 활성탄소제조법을 사용하기 때문에 원료의 손실이 많고 제조비용이 많이 들며 시간도 오래 걸리고 생산효율도 떨어지는 등 결점이 있었다.Conventional activated carbon manufacturing method uses activated carbon manufacturing method of steam regeneration method that carbonizes and adds water, such as coconut shell, fruit peel or grain waste, as raw material, so there is a lot of loss of raw materials, high production cost and time. It also took a long time, and the production efficiency was also poor.
본 발명은 위와 같은 종래의 결점을 시정하기 위하여 발명된 것으로 상세히 설명하면 다음과 같다.The present invention is described in detail as being invented to correct the above conventional drawbacks as follows.
본 발명은 종래의 제조방법과는 판이하게 특정의 구성조건을 갖이고 있는 광유, 즉 방카C유와 같이 탄소함량 85%, 수소함량15%를 함유한 광유를 선택하여 원료로 하고 이에 산화제를 혼합하여 일정온도로 가열하므로서 광유내의 수소가 반응하여 수증기와 SO2가스로 배출되면서 다공체의 탄소가 형성되는 제조방법으로 기존의 제조방법보다 훨신 저렴한 가격으로 큰 활성도를 갖는 제품을 얻게 되는 특징이 있다.The present invention selects mineral oils having a specific constituent condition, that is, mineral oils containing 85% carbon and 15% hydrogen, such as banca C oil, as a raw material and mixing the oxidizing agent with the conventional manufacturing method. By heating to a certain temperature, hydrogen in the mineral oil reacts and is discharged to water vapor and SO 2 gas to form a carbon of the porous body is characterized by obtaining a product having a high activity at a much lower price than the conventional manufacturing method.
특히 본 발명의 원료는 방카C유와 같은 중질유로서 탄소(C35H72)및 수소의 함량비가 85% : 15중량%비를 갖는 광유를 원료로 해서 원료중에 있는 수소를 황산제2철의 산화력으로 반응시켜 물을 만들고 이것을 가열하여 수증기와 아황산가스 상태로 배출시키므로서 다공성의 활성탄소를 제조하는 것이다.In particular, the raw material of the present invention is a heavy oil such as banca C oil as a raw material of carbon (C 35 H 72 ) and mineral oil having a content ratio of 85% to 15% by weight of hydrogen, the hydrogen in the raw material to oxidize ferric sulfate It reacts to make water and heats it and discharges it in the state of water vapor and sulfurous acid gas to produce porous activated carbon.
본 발명에서 지칭하는 방카C유는Banca C oil referred to in the present invention
분자구성 C35H72 Molecular Composition C 35 H 72
분자량 492Molecular Weight 492
탄소함량 85.36%Carbon content 85.36%
수소함량 14.6%로 구성되어 있다.It is composed of 14.6% hydrogen.
이러한 분자구조를 갖는 광유에 황산제2철을 혼합하여 300℃~500℃로 가열하면 원료중의 수소가 산화재와 반응하여 물로 되면서 수증기 및 아황산가스 상태로 배출되고 이로 인해 고순도 다공성인 활성탄소를 제조할수 있다.When ferric sulfate is mixed with mineral oil having such a molecular structure and heated to 300 ° C to 500 ° C, hydrogen in the raw material reacts with the oxidant to become water, and is discharged in the form of water vapor and sulfurous acid gas. It can be manufactured.
한편 본 발명의 제조에 사용된 산화제가 환원된 황산제1철염은 물에 넣어 용해 용출하여 활성탄소와 분리하고 분리된 여액은 여과정제후 공기를 주입시켜 재산화시켜서 황산제2철 염을 만들고 이를 농축하여 황산제2철 1수염 분말을 만들어 재사용하게 된다.Meanwhile, ferrous sulfate with reduced oxidizing agent used in the manufacture of the present invention is dissolved and eluted in water, separated from activated carbon, and the separated filtrate is fertilized by injecting air after filtering and refining to produce ferric sulfate. Concentrate to make ferric sulfate monohydrate powder to reuse.
이것은 아래방정식으로 입증이 된다.This is proved by the equation
황산1철염 2FeSO4+ H2SO4-O2→Ferrous Sulfate 2FeSO 4 + H 2 SO 4- O 2 →
황산2철염 Fe2(SO4)3+ H2O로 합성된다.It is synthesized from ferric sulfate Fe 2 (SO 4 ) 3 + H 2 O.
본 발명의 제조방법에서 얻어지는 반응식의 분자방정식은 다음과 같다.The molecular equation of the reaction scheme obtained in the production method of the present invention is as follows.
황산제2철Ferric sulfate
분자식 Fe2(SO4)3 Molecular formula Fe 2 (SO4) 3
분자량 398Molecular Weight 398
황산제2철 분자해도는 FeSO4+ FeSO4+ SO4… 식으로 표현되며The ferric sulfate molecular diagram is represented by FeSO 4 + FeSO 4 + SO 4 . Expressed as
SO4근의 열분해시에는 SO2+ O2식으로 2 분자가 분해된다.During pyrolysis of SO 4 , 2 molecules are decomposed in the form of SO 2 + O 2 .
즉, Fe2(SO4)3염의 수소와 결합분해시는 2FeSO4+ SO2+ 2H2O의 방정식으로 분해된다.In other words, when combined decomposition with hydrogen of Fe 2 (SO 4 ) 3 salt is decomposed by the equation of 2FeSO 4 + SO 2 + 2H 2 O.
이것이 방카C유와 결합되는 방정식은The equation that combines with banca C oil
18 Fe2(SO4)3+ C35H72→ 36FeSO4+ 18SO2+ 36H2O + 35C18 Fe 2 (SO 4 ) 3 + C 35 H 72 → 36FeSO 4 + 18SO 2 + 36H 2 O + 35C
상기 방정식과 같이 방카C유가 갖고 있는 수소는 모두다 H2O 즉, 물로 변환되고 탄소만 유리되는데 이때의 수소가 빠져나간 구멍이 공간으로 남아 존속하게 되어 다공성 활성탄소를 형성하게 된다.As shown in the above equation, all hydrogens in banca C oil are converted into H 2 O, that is, water, and only carbon is released. At this time, the holes from which hydrogen escapes remain in the space and form porous activated carbon.
상기에서 알수 있듯이 방카C유가 황산제2철염의 산화산소량보다 과다 첨가시에는 산화제2철(Fe2O3) 염을 형성하게 되고 황산제2철 및 황산제2철염의 손실이 발생한다.As can be seen above, when banca C oil is added in excess of the amount of oxygen oxide of ferric sulfate, ferric oxide (Fe 2 O 3 ) salts are formed and loss of ferric sulfate and ferric sulfate occurs.
그 이유는 다음과 같다.The reason for this is as follows.
1. 2FeSO4+ CH2→ FeO3+ 2SO4+ H2O + C1.2FeSO 4 + CH 2 → FeO 3 + 2SO 4 + H 2 O + C
2. Fe2(SO4)3+ C3H6→ FeSO4+ 3SO2+ 3H2O + 3C2.Fe 2 (SO 4 ) 3 + C 3 H 6 → FeSO 4 + 3SO 2 + 3H 2 O + 3C
상기 반응으로 보아서 황산1철, 황산2철염의 손실을 제한하기 위해서는 방카C유가 이론치와 유사한 정량치를 공급해야 한다.In view of the above reaction, in order to limit the loss of ferrous sulfate and ferric sulfate, banca C oil should be supplied with a quantitative value similar to the theoretical value.
즉, 황산제2철염의 총량에 평균 20~25%(중량%)수준에서 방카C유를 첨가하여 열분해 및 탄화시켜 활성탄 제조를 하게된다.That is, banca C oil is added to the total amount of ferric sulfate at an average level of 20 to 25% (wt%) to pyrolyze and carbonize to produce activated carbon.
또 유리황산의 량도 10% 미만인 경우가 바람직하고 황산제2철함수율도 1수염으로 하는 것이 바람직하다.It is also preferable that the amount of free sulfuric acid is less than 10%, and the ferric sulfate content is also preferably monohydrate.
또 방카C유보다 수소함량이 적고 탄소함량이 적은 핏지류와 같은 고탄소함유 유는 활성탄소 생산량은 증가하나 활성도가 떨어진다.In addition, high carbon content such as pit paper containing less hydrogen and less carbon than banca C oil increases the production of activated carbon but decreases its activity.
실 시 예 <1>Example <1>
황산제2철 1수염 [ Fe2(SO4)3H2O ]을 잘 분쇄해서 100메쉬로 만든 1kg을 C35H72상태의 방카C유 25Og 주입혼합하고 가열용기에 넣고 350℃∼500℃로 가열하여 수증기 및 아황산가스(SO2)를 완전 배출시키고 탄화가 완료된 시점에서 물2500cc에 넣고 용출해서 여과분리하고 여액은 황산철용액으로 회수하고 활성탄소 220g를 얻었다.1 kg of ferric sulfate monohydrate [Fe 2 (SO 4 ) 3 H 2 O] finely pulverized into 100 mesh is mixed with 25Og of banca C oil in a C 35 H 72 state and placed in a heating container at 350 ° C to 500 ° C. Water vapor and sulfurous acid gas (SO 2 ) was completely discharged by heating, and when carbonization was completed, the mixture was poured into 2500cc of water, eluted and filtered. The filtrate was recovered with an iron sulfate solution and 220g of activated carbon was obtained.
이렇게 얻은 활성탄소는 시중에서 판매하고 있는 활성탄소보다 활성도가 약1.5배 ~ 2배의 기능이 있음을 역가테스트로 알수가 있었다.The activated carbon obtained in this way was found to have a function of about 1.5 to 2 times higher activity than commercially available activated carbon.
실 시 예 <2>Example <2>
황산제2철 1수염 [ Fe2(SO4)3H2O ] 을 잘분쇄해서 100메쉬로 만든 1kg을 C40H30상태의 아스팔트 30Og을 주입혼합하고 가열용기에 넣고 350℃∼500℃로 가열하여 수증기 및 아황산가스(SO2)를 완전 배출시키고 탄화가 완료된 시점에서 물2500cc에 넣고 용출해서 여과분리하고 여액은 황산철용액으로 회수하고 활성탄소 280g를 얻었다.1 kg of ferrous sulfate monohydrate [Fe 2 (SO 4 ) 3 H 2 O] finely pulverized into 100 mesh was injected and mixed with 30Og of asphalt in a C 40 H 30 state and placed in a heating container at 350 ° C to 500 ° C. After heating, water vapor and sulfurous acid gas (SO 2 ) were completely discharged, and when carbonization was completed, the resultant was poured into 2500cc of water, eluted and filtered. The filtrate was recovered with an iron sulfate solution to obtain 280 g of activated carbon.
본 실험에서는 실시에 1번보다 활성탄소의 여가가 20%감소하였다.In this experiment, the leisure carbon activity was reduced by 20% compared to the first time.
이것은 수소의 량이 아스팔트에서는 부족함으로 활성도가 부족한 것으로 나타났다.It was found that the activity was insufficient because the amount of hydrogen was insufficient in asphalt.
실 시 예 <3>Example <3>
황산제2철 1수염 [ Fe2(SO4)3H2O ] 을 잘분쇄해서 100메쉬로 만든 1kg을 방카C유 150g 경유100g을 주입혼합하고 가열용기에 넣고 350℃∼50O℃까지 가열하여 수증기 및 아황산가스(SO2)를 완전 배출시키고 탄화가 완료된 시점에서 물2500cc에 넣고 용출해서 여과분리하고 여액은 황산철용액으로 회수하고 활성탄소 150g를 얻었다.1 kg of ferric sulfate monohydrate [Fe 2 (SO 4 ) 3 H 2 O] was finely pulverized and 100 kg of banca C oil was mixed with 100 g of diesel oil, and placed in a heating container and heated to 350 ° C. to 50 ° C. Water vapor and sulfurous acid gas (SO 2 ) was completely discharged, and when carbonization was completed, the mixture was poured into 2500cc of water, eluted, filtered, and the filtrate was recovered with an iron sulfate solution to obtain 150g of activated carbon.
이 경우는 경질유가 대부분 증발하고 그 일부가 탄화되므로 350℃~500℃의 온도에서 비증발성 고점도 고카본유의 중질유를 열분해로 사용해야 됨을 입증했다.In this case, since most of the light oil evaporated and a part of it was carbonized, it was proved that pyrolysis of non-evaporable high-viscosity heavy carbon oil at the temperature of 350 ° C to 500 ° C should be used as pyrolysis.
실시예에서 본 결과와 같이 본 발명의 활성탄제조에 사용하는 원료는 C35H72∼ C40H30수준에 있는 고점도 고온에서 탄화되는 중질유를 원료로 사용해야하고 가열온도는 350℃∼500℃에서 완전탄화점으로 해야하는 것을 알수 있었다.As shown in the examples, the raw material used in the production of activated carbon of the present invention should be used as a raw material of heavy oil carbonized at high viscosity high temperature in the level of C 35 H 72 ~ C 40 H 30 and the heating temperature is complete at 350 ℃ ~ 500 ℃ I knew that I should be a carbonization point.
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US9102542B1 (en) * | 2014-02-17 | 2015-08-11 | King Fahd University Of Petroleum And Minerals | Method of producing activated carbon from fuel oil |
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US9102542B1 (en) * | 2014-02-17 | 2015-08-11 | King Fahd University Of Petroleum And Minerals | Method of producing activated carbon from fuel oil |
US20150231603A1 (en) * | 2014-02-17 | 2015-08-20 | King Fahd University Of Petroleum And Minerals | Method of producing activated carbon from fuel oil |
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