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CN1446748A - Method for preparing active carbon with height ratio surface area - Google Patents

Method for preparing active carbon with height ratio surface area Download PDF

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Publication number
CN1446748A
CN1446748A CN 03111949 CN03111949A CN1446748A CN 1446748 A CN1446748 A CN 1446748A CN 03111949 CN03111949 CN 03111949 CN 03111949 A CN03111949 A CN 03111949A CN 1446748 A CN1446748 A CN 1446748A
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China
Prior art keywords
surface area
specific surface
active carbon
activation solution
high specific
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CN 03111949
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Chinese (zh)
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CN1207191C (en
Inventor
谢克昌
曹青
鲍卫仁
吕永康
申暑光
赵彦生
叶俊岭
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Taiyuan University of Technology
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Taiyuan University of Technology
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Publication of CN1446748A publication Critical patent/CN1446748A/en
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Publication of CN1207191C publication Critical patent/CN1207191C/en
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Abstract

An activated carbon with high specific surface area is prepared from corn cob through chirring, treating with molecular osmotic activating liquid, high-temp treating, neutralizing with hydrochloric acid, washing and baking. Its advantages are high specific surface area (2600-2800 sq.m/g) and no environmental pollution.

Description

Active carbon with high specific surface area and preparation method
One, technical field
The present invention is active carbon with high specific surface area and preparation method, belongs to the category of chemical production technical field.
Two, technical background
The gac of preparation high-ratio surface, be not only of the new requirement of departments such as environmental protection, food-processing, meticulous medicine, chemical industry, electronics to this proposition, and be for satisfying of the particular requirement (as hydrogen storage material etc.) of some high-tech area to type material, thereby this class material can more and more be subjected to the attention of high-tech development field, has broad application prospects in development in future.Traditional Preparation of Activated Carbon is a raw material with the shell (as Exocarpium cocois (Cocos nucifera L), spade shell, apricot shell, rice husk) of fruit, coal and the refinery coke that grew up in recent years, pitch etc. usually.In these methods, the method that has is the restriction that is subjected to raw material, causes product price higher; Though the method that has is produced the raw material abundance of gac, because of the limitation that is subjected to method itself and there is severe contamination, the gac specific surface area of production is big inadequately, shortcoming such as lack competitiveness on market.The present invention overcomes the deficiency of this two aspect, has broken conventional employed medicament (as yellow soda ash, zinc chloride, phosphoric acid, potassium hydroxide) on method, used first mention in the claim 2 with tensio-active agent as auxiliary agent.By the lypohydrophilic character of tensio-active agent, realized when tensio-active agent enters the carbide micropore, hydrophilic activator KOH, sodium peroxide are also carried the micropore that has entered carbide thereupon, further brought into play the effect of activator KOH.With used additives is compared, the specific surface area of product is significantly improved; Need not in process of production to add and contain zinc, phosphorus etc. the influential activating substance of environment; The raw material that adopts is that (there is 2.16 * 10 every year in China to a large amount of solid waste corn cobs that produce in the agricultural production process 10Kg), by can prepare the gac of high-specific surface area to the special processing of carbide, improved the utility value of corn cob effectively.Material after this method only needs the molecule infiltration activation solution handled be handled under hot conditions, then under normal temperature environment with hydrochloric acid neutralization, distilled water wash, promptly get product after the oven dry.It is sufficient to have raw materials used source, and the course of processing is simple, and easy handling, required pharmaceutical chemicals are general reagent (cheap), and tooling cost is lower and environmentally friendly, and the specific surface area advantages of higher has realized the purpose of " becoming precious by useless "; That overcome bibliographical information is the low (1500~1600m of gac specific surface area that raw material production goes out with the corn cob 2/ g), the drawback of complex process, have a extensive future.
Three, summary of the invention
A kind of active carbon with high specific surface area is characterized in that being is raw material with the agricultural wastes corn cob, adopts the molecule infiltration activation solution to handle the prepared gac of method of carbide, and specific surface area is 2600~2800m 2/ g, pore size distribution is narrow, and wherein, the micropore of aperture below 10nm accounts for 90%, and pore volume is 0.06~0.6cm 3/ g.The molecule infiltration activation solution is made up of auxiliary agent and promoting agent, auxiliary agent is made up of kinds of surface promoting agent JFC, MP, soap etc., promoting agent is made up of sodium peroxide and KOH, its corresponding weight percent JFC, MP, soap, sodium peroxide, potassium hydroxide are 0.01~0.03: 0.015~0.02: 0.01~0.015: 0.03~0.08: 0.5~5: 0.8~15, and other is a solvent.During preparation JFC, MP, soap, sodium peroxide, potassium hydroxide material (no sequencing) are placed in the bigger glass or plastic containers; add required solvent distilled water; stir with glass stick and to get final product; raw material is under protection of nitrogen gas; handle the back through charing and carry out osmotic treated with the molecule infiltration activation solution, oven dry, high-temperature activation, pickling, to dry be key step again.Its concrete processing step is as follows: after the oven dry of (1) raw material corn cob, pulverize, its granularity should be in 40~120 order scopes.(2) with nitrogen as protection gas, under 350 ℃~500 ℃ temperature, carry out charing and handle 2~5h.(3) carry out saturation process 2~6h with the molecule infiltration activation solution, oven dry.(4) with nitrogen as the protection gas, activation treatment 1~2h under 700~850 ℃ condition.(5) use 3molL -1The product washing of hydrochloric acid soln after will activating to neutral, with 60~70
℃ distilled water rinsing after heat filter.(6) bake out temperature is 110~120 ℃, and the time is 8~12h.
Four, embodiment
Mode 1. is crushed to 60 purpose solid waste corn cobs with 1Kg and puts into charring furnace, feeding under the condition of nitrogen in 450 ℃ temperature charing 4h, activation solution dipping 2h is soaked into molecule in the cooling back, activation solution is formulated in bigger plastic containers under the effect that glass stick stirs by 0.03Kg JFC, 0.02KgMP, 0.01Kg soap, 0.03Kg sodium peroxide, 3.5Kg potassium hydroxide and 0.8Kg distilled water, and the carbide drying behind the dipping is put into the high-temperature activation stove, the controlled temperature that are connected with the nitrogen existence and activate 1h under 800 ℃ condition; Take out the cooling back, uses 3molL -1Chlorohydric acid pickling to neutral, add temperature again and be 60 ℃ hot distilled water rinsing, heat filter, under 120 ℃ condition, dry by the fire 8h, can get specific surface area 2800m 2The high grade activated carbon of/g.
Mode 2. is crushed to 40 purpose solid waste corn cobs with 1Kg and puts into charring furnace, feeding under the condition of nitrogen in 500 ℃ temperature charing 4h, activation solution dipping 4h is soaked into molecule in the cooling back, activation solution is formulated in bigger plastic containers under the effect that glass stick stirs by 0.03Kg JFC, 0.02KgMP, 0.012Kg soap, 0.05Kg sodium peroxide, 4.5Kg potassium hydroxide and 0.8Kg distilled water, and the carbide drying behind the dipping is put into and is connected with nitrogen and has the high-temperature activation stove, be to activate 1h under 800 ℃ the condition in temperature; Take out the cooling back, uses 3molL -1Chlorohydric acid pickling to neutral, add temperature again and be 70 ℃ hot distilled water rinsing, heat filter, under 120 ℃ condition, dry by the fire 10h, can get specific surface area 2780m 2The high grade activated carbon of/g.Mode 3. is crushed to 120 purpose solid waste corn cobs with 1Kg and puts into charring furnace, feeding under the condition of nitrogen in 400 ℃ temperature charing 4h, activation solution dipping 3h is soaked into molecule in the cooling back, activation solution is formulated in bigger plastic containers under the effect that glass stick stirs by 0.025Kg JFC, 0.015KgMP, 0.012Kg soap, 0.05Kg sodium peroxide, 5Kg potassium hydroxide and 0.8Kg distilled water, and the carbide drying behind the dipping is put into and is connected with nitrogen and has the high-temperature activation stove, be to activate 1h under 800 ℃ the condition in temperature; Take out the cooling back, uses 3molL -1Chlorohydric acid pickling to neutral, add temperature again and be 70 ℃ hot distilled water rinsing, heat filter, under 120 ℃ condition, dry by the fire 10h, can get specific surface area 2680m 2The high grade activated carbon of/g.

Claims (4)

1. active carbon with high specific surface area is characterized in that being is raw material with the agricultural wastes corn cob, adopts the molecule infiltration activation solution to handle the prepared gac of method of carbide, and specific surface area is 2600~2800m 2/ g, pore size distribution is narrow, and wherein, the micropore of aperture below 10nm accounts for 90%, and pore volume is 0.06~0.6cm 3/ g.
2. according to the described method for preparing active carbon with high specific surface area of claim 1, it is characterized in that adopting the molecule infiltration activation solution to handle carbide, its molecule infiltration activation solution is made up of auxiliary agent and promoting agent, wherein, auxiliary agent is made up of kinds of surface promoting agent JFC, MP, soap etc., and promoting agent is made up of sodium peroxide and KOH; Its weight percent JFC, MP, soap, sodium peroxide, potassium hydroxide are: 0.01~0.03: 0.015~0.02: 0.01~0.015: 0.03~0.08: 0.5~5: 0.8~15, and other is a solvent.As long as JFC, MP, soap, sodium peroxide, potassium hydroxide material (no sequencing) are placed in the bigger glass or plastic containers, add required solvent during preparation, stirring with glass stick gets final product, and concrete operations step and processing parameter are as follows:
(1) after the oven dry of raw material corn cob, pulverize, its granularity is in 40~120 order scopes.
(2) with nitrogen as protection gas, under 350 ℃~500 ℃ temperature, carry out charing and handle
2~5h。
(3) carry out saturation process 2~6h with the molecule infiltration activation solution, oven dry.With nitrogen as the guarantor
Protect gas, activation treatment 1~2h under 700~850 ℃ condition.
(4) use 3molL -1The product of hydrochloric acid soln after will activating wash to neutrality, use
60~70 ℃ of distilled water rinsing after heat filters.
(5) bake out temperature is 110~120 ℃, and the time is 8~12h.
3. described according to claim 1 is the feedstock production active carbon with high specific surface area with the agricultural wastes corn cob, it is characterized in that raw materials used granularity is 40~120 orders.
4. according to the described method for preparing active carbon with high specific surface area of claim 2, the solvent that it is characterized in that preparing the molecule infiltration activation solution is a distilled water.
CN 03111949 2003-03-07 2003-03-07 Method for preparing active carbon with height ratio surface area Expired - Fee Related CN1207191C (en)

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Application Number Priority Date Filing Date Title
CN 03111949 CN1207191C (en) 2003-03-07 2003-03-07 Method for preparing active carbon with height ratio surface area

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Application Number Priority Date Filing Date Title
CN 03111949 CN1207191C (en) 2003-03-07 2003-03-07 Method for preparing active carbon with height ratio surface area

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CN1446748A true CN1446748A (en) 2003-10-08
CN1207191C CN1207191C (en) 2005-06-22

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100337911C (en) * 2005-01-27 2007-09-19 西北农林科技大学 Method for producing active carbon by using straw mixed raw material
CN100434361C (en) * 2007-03-12 2008-11-19 陈温福 Simply corncob granule carbonization furnace and preparation method thereof
CN100467372C (en) * 2007-04-05 2009-03-11 吉林大学 Method of preparing biomass high specific surface micro-pore carbon material
CN102275911A (en) * 2011-06-03 2011-12-14 中国林业科学研究院林产化学工业研究所 Microporous active carbon and preparation method by chemical agent aperture regulation and control
CN102774837A (en) * 2012-08-15 2012-11-14 福建农林大学 Method for preparing activated carbon by taking ionic liquid as activator
CN104888708A (en) * 2015-07-02 2015-09-09 黑龙江大学 Corn bran-based three-dimensional multi-level pore structure carbon material and preparation method thereof
CN111785535A (en) * 2020-08-04 2020-10-16 山东理工大学 Preparation method of self-activated high-specific-capacitance carbon nanotube electrode
CN112979219A (en) * 2021-03-16 2021-06-18 浙江理工大学 Porous carbon fiber material with photo-thermal and joule-thermal essential oil controlled release functions and preparation method thereof
CN113120902A (en) * 2019-12-31 2021-07-16 中国石油化工股份有限公司 Preparation method of activated carbon

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100337911C (en) * 2005-01-27 2007-09-19 西北农林科技大学 Method for producing active carbon by using straw mixed raw material
CN100434361C (en) * 2007-03-12 2008-11-19 陈温福 Simply corncob granule carbonization furnace and preparation method thereof
CN100467372C (en) * 2007-04-05 2009-03-11 吉林大学 Method of preparing biomass high specific surface micro-pore carbon material
CN102275911A (en) * 2011-06-03 2011-12-14 中国林业科学研究院林产化学工业研究所 Microporous active carbon and preparation method by chemical agent aperture regulation and control
CN102774837A (en) * 2012-08-15 2012-11-14 福建农林大学 Method for preparing activated carbon by taking ionic liquid as activator
CN104888708A (en) * 2015-07-02 2015-09-09 黑龙江大学 Corn bran-based three-dimensional multi-level pore structure carbon material and preparation method thereof
CN104888708B (en) * 2015-07-02 2017-06-27 黑龙江大学 Corn scytoblastema three-dimensional multistage pore structure carbon material and preparation method thereof
CN113120902A (en) * 2019-12-31 2021-07-16 中国石油化工股份有限公司 Preparation method of activated carbon
CN113120902B (en) * 2019-12-31 2022-11-11 中国石油化工股份有限公司 Preparation method of activated carbon
CN111785535A (en) * 2020-08-04 2020-10-16 山东理工大学 Preparation method of self-activated high-specific-capacitance carbon nanotube electrode
CN112979219A (en) * 2021-03-16 2021-06-18 浙江理工大学 Porous carbon fiber material with photo-thermal and joule-thermal essential oil controlled release functions and preparation method thereof
CN112979219B (en) * 2021-03-16 2022-08-23 浙江理工大学 Porous carbon fiber material with photo-thermal and joule-thermal essential oil controlled release functions and preparation method thereof

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