CN107188172B - A kind of preparation method rich in mesoporous pitch super active carbon - Google Patents
A kind of preparation method rich in mesoporous pitch super active carbon Download PDFInfo
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- CN107188172B CN107188172B CN201710505340.3A CN201710505340A CN107188172B CN 107188172 B CN107188172 B CN 107188172B CN 201710505340 A CN201710505340 A CN 201710505340A CN 107188172 B CN107188172 B CN 107188172B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
Abstract
A kind of preparation method rich in mesoporous pitch super active carbon is to crush carbon raw material, be sieved into 80-200 mesh powder, it is directly mixed with activator KOH and low boiling point organic solvent, surfactant, it is passed through nitrogen or argon gas, continuously into reaction system with 2-10oThe heating rate of C/min is to 600-770oC activation temperature simultaneously keeps the temperature 1-3h, with the KOH and K of water dissolution wash residual after discharging2O, realizes the recycling of activator, and product is washed, dry to get the super-activated carbon for being rich in mesoporous.The advantages of present invention has simple process, and KOH dosage is few, high surface area and high proportion mesoporous.
Description
Technical field
The present invention relates to a kind of preparation methods of active carbon, are rich in mesoporous asphaltic base super-active more particularly to one kind
The preparation method of charcoal.
Background technique
Active carbon is widely used due to its biggish specific surface area, pore structure abundant and stable chemical property
In traditional chemical field such as gas separation, air cleaning, sewage treatment and catalyst carrier.In recent years, with electrotechnical, electronic, essence
The demand refined in work and the high frontier such as clean energy resource and aerospace to high performance active carbon is increasingly strong, specific surface area
For 800-1500 m2The normal activated carbon of/g is limited due to its adsorption capacity, it is difficult to meet the above new application requirement, thus open
Hair specific surface area reaches 2000 m2The super-activated carbon of/g or more becomes the hot spot in porous carbon material research field.
The raw material for preparing super-activated carbon is generally coal, pitch coke, petroleum coke, shell, resin etc., preparation (activation) side
Method is broadly divided into two classes: i.e. physical activation method and chemical activation method.The former will contain carbon matrix precursor charing first, and removing is therein can
Volatile ingredient generates the pyrolysis object of rich carbon, then passes to ammonium hydroxide or oxidizing gas (such as vapor, air and titanium dioxide
Carbon), by carrying out aperture, reaming to presoma and creating new bore, form flourishing microcellular structure.And chemical activation method generally needs
Chemical activation reagent is added (such as: KOH, NaOH, ZnCl2、CaCl2、H3PO4、H2SO4Deng) to raw material presoma or in advance charing after
Raw material activated to obtain super-activated carbon.Although physical-chemical can also be used in the research in relation to preparing super-active
The method or other methods combined, such as template, but due to process complexity, template higher cost and recycling difficulty, it produces
Product specific surface area is less high, therefore its industrial value is little.
Currently, preparing active carbon with high specific surface area effect the best way is KOH chemical activation method.Patent CN
101209839A uses KOH for activator, in alkali carbon ratio less than 6 and 800-950oCoal is activated under C, obtains specific surface
Up to 3460 m2The high performance active carbon of/g.It is worth noting that, the activation temperature of KOH is logical in such method of open report
Often 800oC or more has a large amount of potassium steam in the process and generates.And potassium is a kind of very active metal simple-substance, it meets
Moisture into air can react displacing hydrogen, and release a large amount of heat, even result in explosion.Meanwhile potassium steam
During evolution, part meeting cold junction is in the pipeline of activation equipment, so that blocking pipeline, can also bring hidden to safety in production
Suffer from.It therefore, is to solve the safety of KOH activation process using the key technology of KOH activation method production super-activated carbon.Existing one
The relevant processing method of a little patent reports or device such as CN 101993071A, CN 106587058A, CN 101058420A,
CN 101434389A,CN 106587058A,CN 101468797A.But above method be mixed into advance assistant activator or
Alcohol reagent is added at high temperature or activation furnace is put into the melting pot, these processes increase process complexity, work invariably
Skill condition is difficult to control, or even there are potential risks, is also unfavorable for industrializing continuous production.
In addition to this, activation temperature is reduced, makes it 800oC is activated below or a reduction potassium steam largely escapes
Method, but rarely have related patents and document report, the reduction of activation temperature may will affect activation effect after all.It is carbon containing to make
Presoma sufficiently activates at a lower temperature and is converted into super-activated carbon, this just needs to carry out presoma selection and to tradition
Activating pretreatment mode improve.
On the other hand, other than specific surface area, the research of pore-size distribution and its regulation to active carbon is also current charcoal
The forward position of investigation of materials.Regulation is oriented to its pore structure while preparing active carbon with high specific surface area, is not only facilitated
Active carbon theoretical system it is abundant and perfect, and facilitate the professional application field for further widening active carbon.Currently, super
Seldom its pore-size distribution is regulated and controled in the research of active carbon.Its pass is mostly in super-activated carbon obtained by aforementioned patent
Pore type duct, mesoporous proportion (2-50nm of aperture) are seldom.In fact, mesopore activated carbon because have biggish aperture and
Kong Rong makes it be more suitable for the liquid phase adsorptions such as natural macromolecular pigment in catalyst and pharmaceutical carrier, fermentation liquid.Therefore, it needs to make
The standby super-activated carbon for being rich in mesoporous.Patent CN 102139875A carries out processing to raw material first and prepares with flourishing big
Then the absorbent charcoal material in hole and central hole structure activates it using modifying supercritical technical matters, further pore-creating, final to make
Obtain super-activated carbon.In the method, by pretreatment be introduced into the feed in advance in macropore, but micro content is still inclined in product
Height, technique are also rather complicated.Patent CN 101028923A waves it easily first through pre-oxidation treatment using petroleum coke class raw material
It sends out substance oxidation and burns mistake, being formed has the pre-oxidation of certain porosity burnt, then will pre-oxidize burnt and alkali metal hydrogen in mass ratio
Oxide is uniformly mixed, and carries out high-temperature activation under an inert atmosphere.Patent CN 1915808A is then first progress reduced pressure treatment removing
In raw material after volatile matter, then super-activated carbon is prepared in the activation that heats up.After the above patent tool is first removes the volatile matter in raw material
Reactivation, products obtained therefrom still contain a high proportion of micropore, and there is also complicated multisteps and process conditions harshness etc. for preparation process
Disadvantage.Although also being referred to after directly mixing KOH with petroleum coke in patent CN 1304788A, it is warming up to 400oC stops 1h,
Finally 800oIt is activated under C, products obtained therefrom specific surface area is more than 3500m2/ g, but KOH amount used is big (alkali charcoal ratio 5:1), causes to produce
Product higher cost.And there are still security risks caused by the evolution of potassium simple substance.
Summary of the invention
It is endangered for the potassium steam for preparing generation present in super-activated carbon technique at present, process flow is complicated, product
The problems such as micropore is excessive, the purpose of the present invention propose a kind of simple process, and KOH dosage is few, high surface area and high proportion mesoporous
Preparation method rich in mesoporous pitch super active carbon.
Under normal conditions, when total pore volume is identical, the increase of mesoporous may result in the decline of specific surface area.High surface
Long-pending and a high proportion of mesopore content is difficult to get both, this proposes challenge for the preparation of the super-activated carbon rich in mesoporous.To solve
The pitch of this problem, the 5-70% that the present invention selects toluene insolubles (TI) component to account for its total weight first is raw material, does not remove it
In volatile matter, compared with low activation temperature (be not higher than 770oC straight by using KOH) and in the presence of surfactant
Taking over a job pitch generates more active channel by volatile matter in activation process, improves activation effect, reduces reaction energy
Consumption obtains the super-activated carbon rich in mesoporous.The present invention is compared with other methods, and it is a series of both to have solved high-temperature operation bring
Problem decreases the dosage and energy consumption of activator KOH.
Preparation method of the invention includes the following steps:
Carbon raw material is crushed, is sieved into 80-200 mesh powder, by itself and activator KOH and low boiling point organic solvent, table
Face activating agent directly mixes, and nitrogen or argon gas are continuously passed through into reaction system.With 2-10oThe heating rate of C/min is extremely
600-770oC activation temperature simultaneously keeps the temperature 1-3h, with the KOH and K of water dissolution wash residual after discharging2O realizes returning for activator
It receives, product is washed, dries to get the super-activated carbon of mesoporous is rich in, wherein the weight proportion of carbon raw material and activator KOH
For 1:1.5-3, the weight ratio of low boiling point organic solvent and carbon raw material is 0.01-0.05:1, surfactant and carbon containing original
The weight ratio of material is 0.005-0.03.
As described above, carbon raw material includes one or more of asphalt, coal tar pitch, bitumen mixture, and
Toluene insolubles (TI) component accounts for the 5-70% of its total weight in above-mentioned asphalt stock.
As described above, the weight proportion of carbon raw material and activator KOH are preferably 1:2.5-3.
As described above, low boiling point organic solvent includes methanol, ethyl alcohol, acetone, one in n,N-Dimethylformamide (DMF)
Kind is several, and the weight ratio of low boiling point organic solvent and carbon raw material is preferably 0.02-0.03:1.
As described above, surfactant includes polyvinyl alcohol, fatty acid sorbitan (sapn), in polysorbate (tween)
One or more, and the weight ratio of added surfactant and carbon raw material is preferably 0.01-0.02.
As described above, activation temperature is preferably 680-750oC。
The advantage of the method for the present invention compared with prior art is:
1) raw material is converted into active carbon through step charcoal activation, one pot of whole process completion, saves material transfer,
Easy to operate and suitable industrialization continuous production；
2) traditional impregnating agent (water) is replaced using low boiling point organic solvent, and dosage is few, volatilization is fast, avoids dry for a long time
Dry dehydration, and the addition of surfactant substantially increases contact effect of the KOH with pitch, improves activation efficiency；
3) activation temperature of the present invention is lower, is 600~770 DEG C, reduces energy consumption, reduce the requirement to equipment；
4) since reaction temperature is lower than the boiling point of potassium vapor, therefore the evolution of metallic potassium steam is avoided；
5) super-activated carbon prepared by, 2500 m of BET specific surface area2/ g or more, Kong Rong are higher than 1.25 cm3/ g mesoporous
Proportion increases its functional suction-operated, forms the unique purposes of active carbon up to 50% or more.
Specific embodiment
The method of the present invention will be described further by several embodiments below.
Embodiment 1
It will be crushed containing the coal tar pitch that TI is 45wt%, be sieved into 80 mesh powder, then stirred with KOH, ethyl alcohol, polyvinyl alcohol
Mixing, coal tar pitch: KOH: ethyl alcohol: polyvinyl alcohol weight ratio 1:3:0.03:0.02 is continuously passed through nitrogen into reaction system,
With 2oThe heating rate of C/min is to 750oC simultaneously keeps the temperature 1h.With the KOH and K of water dissolution wash residual after discharging2O realizes activator
Recycling.Product is washed, dry to get the super-activated carbon for being rich in mesoporous.Its BET specific surface area is 3421m2/ g, Kong Rong
For 1.95 cm3/ g, mesoporous 51%.
Embodiment 2
It will be crushed containing the coal tar pitch that TI is 70wt%, be sieved into 100 mesh powder, it is then mixed with KOH, methanol, sapn stirring
Close, coal tar pitch: KOH: methanol: sapn weight ratio is 1:1.5:0.01:0.005, and nitrogen is continuously passed through into reaction system.With
3oThe heating rate of C/min is to 600oC simultaneously keeps the temperature 3h.With the KOH and K of water dissolution wash residual after discharging2O realizes activator
Recycling.Product is washed, dry to get the super-activated carbon for being rich in mesoporous.Its BET specific surface area is 2740 m2/ g, Kong Rongwei
1.25 cm3/ g, mesoporous 62%.
Embodiment 3
It will be crushed containing the asphalt that TI is 5wt%, be sieved into 200 mesh powder, it is then mixed with KOH, acetone, tween stirring
Close, asphalt: KOH: acetone: tween weight ratio is 1:2.5:0.05:0.01, and nitrogen is continuously passed through into reaction system.With
10oThe heating rate of C/min is to 770oC simultaneously keeps the temperature 2h.With the KOH and K of water dissolution wash residual after discharging2O realizes activator
Recycling.Product is washed, dry to get the super-activated carbon for being rich in mesoporous.Its BET specific surface area is 2823m2/ g, Kong Rong
For 1.65 cm3/ g, mesoporous 60%.
Embodiment 4
Will containing TI be 37wt% bitumen crush, be sieved into 80 mesh powder, then with KOH, DMF, polyvinyl alcohol, spit
Temperature is stirred, bitumen: KOH:DMF: polyvinyl alcohol: tween weight ratio is 1:1.8:0.05:0.005:0.005, to anti-
It answers and is continuously passed through argon gas in system.With 5oThe heating rate of C/min is to 700oC simultaneously keeps the temperature 2.5h.It is residual with water dissolution washing after discharging
The KOH and K stayed2O realizes the recycling of activator.Product is washed, dry to get the super-activated carbon for being rich in mesoporous.Its BET
Specific surface area is 2954m21.65 cm of/g, Kong Rongwei3/ g, mesoporous 58%.
Embodiment 5
By be 25wt% containing TI coal tar pitch and containing TI be 37wt% bitumen crush, be sieved into 200 mesh powder, then
Be stirred with KOH, ethyl alcohol, sapn, coal tar pitch: bitumen: KOH: ethyl alcohol: sapn weight ratio is 1:1:6:0.06:0.06,
Nitrogen is continuously passed through into reaction system.With 5oThe heating rate of C/min is to 700oC simultaneously keeps the temperature 1h.It is dissolved and is washed with water after discharging
Remaining KOH and K2O realizes the recycling of activator.Product is washed, dry to get the super-activated carbon for being rich in mesoporous.Its
BET specific surface area is 3022m21.76 cm of/g, Kong Rongwei3/ g, mesoporous 55%.
Embodiment 6
By be 64wt% containing TI coal tar pitch and containing TI be 5wt% asphalt crush, be sieved into 100 mesh powder, then
It is stirred with KOH, methanol, ethyl alcohol, polyvinyl alcohol, coal tar pitch: asphalt: KOH: methanol: ethyl alcohol: polyvinyl alcohol weight ratio
For 2:1:7.5:0.05:0.05:0.09, nitrogen is continuously passed through into reaction system.With 6oThe heating rate of C/min is to 650oC is simultaneously
Keep the temperature 3h.With the KOH and K of water dissolution wash residual after discharging2O realizes the recycling of activator.Product is washed, it is dry to get
Super-activated carbon rich in mesoporous.Its BET specific surface area is 2657m21.46 cm of/g, Kong Rongwei3/ g, mesoporous 61%.
Embodiment 7
By be 37wt% containing TI bitumen and containing TI be 5wt% asphalt crush, be sieved into 100 mesh powder, so
It is stirred afterwards with KOH, acetone, polyvinyl alcohol, tween, bitumen: asphalt: KOH: acetone: polyvinyl alcohol: tween weight
Amount is continuously passed through argon gas into reaction system than being 1:2:9:0.06:0.005:0.01.With 10oThe heating rate of C/min is extremely
680oC simultaneously keeps the temperature 1.5h.With the KOH and K of water dissolution wash residual after discharging2O realizes the recycling of activator.Product is washed,
Drying is to get the super-activated carbon for being rich in mesoporous.Its BET specific surface area is 3017 m21.66 cm of/g, Kong Rongwei3/ g, mesoporous
It is 57%.
Embodiment 8
By be 64wt% containing TI coal tar pitch and containing TI be 37wt% bitumen crush, be sieved into 80 mesh powder, then
Be stirred with KOH, ethyl alcohol, sapn, tween, coal tar pitch: bitumen: KOH: ethyl alcohol: sapn: tween weight ratio is 3:1:9:
0.05:0.04:0.02 is continuously passed through nitrogen into reaction system.With 5oThe heating rate of C/min is to 750oC simultaneously keeps the temperature 1h.Out
With the KOH and K of water dissolution wash residual after material2O realizes the recycling of activator.Product is washed, dry to get rich in mesoporous
Super-activated carbon.Its BET specific surface area is 3227m21.81 cm of/g, Kong Rongwei3/ g, mesoporous 56%.
Embodiment 9
By be 25wt% containing TI coal tar pitch, containing TI be 5% asphalt and containing TI be 37% bitumen crush, sieve
It is divided into 80 mesh powder, is then stirred with KOH, ethyl alcohol, sapn, tween, coal tar pitch: asphalt: bitumen: KOH: second
Alcohol: sapn: tween weight ratio is 2:1:1:8:0.05:0.04:0.02, and nitrogen is continuously passed through into reaction system.With 8oC/min
Heating rate to 700oC simultaneously keeps the temperature 1.5h.With the KOH and K of water dissolution wash residual after discharging2O realizes the recycling of activator.
Product is washed, dry to get the super-activated carbon for being rich in mesoporous.Its BET specific surface area is 3347 m2/ g, Kong Rongwei 1.98
cm3/ g, mesoporous 51%.
Above description sufficiently discloses a specific embodiment of the invention.It should be pointed out that pitch in the present invention
Toluene insolubles (TI) component accounts for the 5-70% of its total weight in raw material, for this purpose, its modulation means includes but is not limited to be catalyzed pyrocondensation
Poly-, air oxidation, nitrogen purging, extraction, extract back-mixing etc..One skilled in the art is to specific implementation of the invention
Any change that mode is done all without departing from claims of the present invention range, correspondingly, claim of the invention
Range is also not limited only to previous embodiment.
Claims (8)
1. a kind of preparation method rich in mesoporous pitch super active carbon, it is characterised in that include the following steps:
Carbon raw material is crushed, is sieved into 80-200 mesh powder, it is lived with activator KOH and low boiling point organic solvent, surface
Property agent directly mixes, and nitrogen or argon gas are continuously passed through into reaction system；
With 2-10oThe heating rate of C/min is to 600-770oC activation temperature simultaneously keeps the temperature 1-3h, is dissolved and is washed with water after discharging
Remaining KOH and K2O realizes the recycling of activator, and product is washed, dry to get the super-activated carbon for being rich in mesoporous, wherein
The weight proportion of carbon raw material and activator KOH are 1:1.5-3, and the weight ratio of low boiling point organic solvent and carbon raw material is
The weight ratio of 0.01-0.05:1, surfactant and carbon raw material is 0.005-0.03；
The carbon raw material is one or more of asphalt, coal tar pitch, bitumen mixture.
2. a kind of preparation method rich in mesoporous pitch super active carbon as described in claim 1, it is characterised in that: pitch
Toluene insolubles component accounts for the 5-70% of its total weight in raw material.
3. a kind of preparation method rich in mesoporous pitch super active carbon as described in claim 1, it is characterised in that described
The weight proportion of carbon raw material and activator KOH are 1:2.5-3.
4. a kind of preparation method rich in mesoporous pitch super active carbon as described in claim 1, it is characterised in that described
Low boiling point organic solvent includes one or more of methanol, ethyl alcohol, acetone, N,N-dimethylformamide.
5. a kind of preparation method rich in mesoporous pitch super active carbon as described in claim 1, it is characterised in that described
Low boiling point organic solvent and carbon raw material weight ratio be 0.02-0.03:1.
6. a kind of preparation method rich in mesoporous pitch super active carbon as described in claim 1, it is characterised in that described
Surfactant is one or more of polyvinyl alcohol, fatty acid sorbitan, polysorbate.
7. a kind of preparation method rich in mesoporous pitch super active carbon as described in claim 1, it is characterised in that described
Surfactant and carbon raw material weight ratio be 0.01-0.02.
8. a kind of preparation method rich in mesoporous pitch super active carbon as described in claim 1, it is characterised in that described
Activation temperature is 680-750oC。
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| CN110627064B (en) * | 2018-06-22 | 2022-08-05 | 中南大学 | Method for preparing nitrogen-doped activated carbon material by using plant asphalt as raw material |
| CN109133055A (en) * | 2018-08-03 | 2019-01-04 | 山西煤炭进出口集团科学技术研究院有限公司 | A kind of preparation method and application of high-purity medium temperature coal pitch super active carbon |
| CN108910881A (en) * | 2018-08-27 | 2018-11-30 | 天津市职业大学 | A kind of composite activating agent preparing high performance active carbon and its application |
| CN110127694A (en) * | 2019-05-17 | 2019-08-16 | 中国铝业股份有限公司 | A kind of preparation method of asphalt based active carbon |
| CN114715970A (en) * | 2022-03-31 | 2022-07-08 | 延安大学 | Method for removing glyphosate in water through adsorption of porous carbon material of coal tar pitch substrate layer |
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| JP2004534713A (en) * | 2001-07-13 | 2004-11-18 | ケント ステイト ユニバーシティ | Imprinted mesoporous carbon and method for producing the same |
| JP2006347864A (en) * | 2005-05-19 | 2006-12-28 | Mitsubishi Gas Chem Co Inc | Method for producing mesoporous carbon, and mesoporous carbon |
| CN100396608C (en) * | 2006-09-15 | 2008-06-25 | 江苏工业学院 | Method of preparing high specific surface area activated carbon with rich mesoporous |
| CN101844765B (en) * | 2010-06-02 | 2012-01-11 | 天津大学 | Active carbon for preparing carbon electrode of super capacitor and preparation method thereof |
| CN102431992B (en) * | 2011-09-22 | 2013-07-24 | 安徽工业大学 | Method for preparing porous carbon material by using magnesium oxide template in cooperation with activation of potassium hydroxide |
| CN104264285A (en) * | 2014-09-25 | 2015-01-07 | 四川创越炭材料有限公司 | Method for preparing mesoporous activated carbon fibers |
| CN104261406B (en) * | 2014-09-25 | 2016-01-20 | 四川创越炭材料有限公司 | A kind of asphaltic base mesopore spheric active carbon and preparation method thereof |
| CN104591184A (en) * | 2015-02-03 | 2015-05-06 | 安徽工业大学 | Preparation method of shell-like mesoporous carbon material for super capacitors |
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