CN106554014A - A kind of method that self-activation method prepares activated carbon - Google Patents
A kind of method that self-activation method prepares activated carbon Download PDFInfo
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- CN106554014A CN106554014A CN201611064899.9A CN201611064899A CN106554014A CN 106554014 A CN106554014 A CN 106554014A CN 201611064899 A CN201611064899 A CN 201611064899A CN 106554014 A CN106554014 A CN 106554014A
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- activated carbon
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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
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
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Abstract
The present invention relates to a kind of method that self-activation method prepares activated carbon, methods described includes for biological raw material carrying out the pretreated feedstock that pulverization process obtains 60 300 mesh；Pretreated feedstock Jing temperature programmings after being warming up to 800 1200 DEG C of activation temperature with the heating rate of 10 100 DEG C/min, then intermediate product is obtained after carrying out 5 10h of activation process；The intermediate product is carried out cooling treatment to take out to default chilling temperature, that is, specific surface area is obtained more than 1100m2The activated carbon product of/g.Self-activation method proposed by the present invention prepares the method for activated carbon in preparation process without the need for chemical reagent, without being post-processed, step is relatively simple, improves the preparation quality and production efficiency of activated carbon, the preparation cost of activated carbon is reduced, is had a good application prospect.
Description
Technical field
The present invention relates to activated carbon preparing technical field, the method that more particularly to a kind of self-activation method prepares activated carbon.
Background technology
Activated carbon is a kind of excellent sorbing material, as which has the pore structure of prosperity, larger specific surface area, good
The advantageous property such as good electric conductivity and chemical stability, national defence, chemical industry, oil, weaving, food, medicine, transportation and energy,
The every field such as agricultural, urban construction, atomic energy industry suffer from extensive purposes.
The existing method for preparing activated carbon is roughly divided into three classes：(1) physical activation method：Physical activation method is generally divided into charcoal
Change and activate two steps, carry out charing dehydration first by presoma at a certain temperature and form carbide, then pass to oxidisability
Which is made to react the pore structure to form prosperity with carbide at high temperature in gas.Wherein conventional oxidizing gas have CO2、H2O
Or O2.(2) chemical activation method：Chemical activation method also includes carbonizing and activates two processes, and the two processes can be carried out simultaneously
Can also carry out step by step.Chemical activation method is the inside by the mode such as activator soaking to be penetrated into presoma, after drying
Heat up carbonization and activation are carried out in an inert atmosphere, it is with the chemical reagent remained in sour clean-out opening after the completion of activation, final to be obtained
Activated carbon.Wherein there is H using the chemical activating agent of more and comparative maturity at present3PO4And KOH etc..(3) physical chemistry activation
Method：Physical chemistry activation method is physical activation method and chemical activation method is used in combination.
In the actual fabrication process of current activated carbon, due to general higher using the temperature needed for physical activation method,
Required soak time is also longer, consumes energy larger, and the yield of activated carbon is relatively low；And adopt analysis for preparation of activated carbon by chemical activation pair
The corrosivity of equipment is larger, and step is relatively complicated, and causes production cost higher the problems such as be not easily recycled.It is therefore desirable to proposing
A kind of new method of relatively succinct, environmental protection is preparing activated carbon to meet the needs of current social development and application.
The content of the invention
Based on this, it is an object of the invention to provide a kind of relatively easy, environmentally friendly method for preparing activated carbon is preparing work
Property charcoal, to meet the demand of production application.
The present invention proposes a kind of method that self-activation method prepares activated carbon, comprises the following steps：
Biological raw material is carried out into the pretreated feedstock that pulverization process obtains 60-300 mesh；
Pretreated feedstock Jing temperature programmings are simultaneously warming up to 800-1200 DEG C with the heating rate of 10-100 DEG C/min
After activation temperature, then intermediate product is obtained after carrying out activation process 5-10h；
The intermediate product is carried out cooling treatment to take out to default chilling temperature, that is, is obtained specific surface area and is more than
1100m2The activated carbon product of/g.
The method that the self-activation method prepares activated carbon, wherein, the biological raw material is stalk, bagasse or peanut shell.
The method that the self-activation method prepares activated carbon, wherein, the particle size of the pretreated feedstock is 60 mesh, 80 mesh
Or 100 mesh.
The method that the self-activation method prepares activated carbon, wherein, the heating rate is 30 DEG C/min or 50 DEG C/min.
The method that the self-activation method prepares activated carbon, wherein, the activation temperature is 900 DEG C, 950 DEG C or 1000 DEG C.
The method that the self-activation method prepares activated carbon, wherein, carry out the activation process time be 2.5h, 3h or
4h。
The method that the self-activation method prepares activated carbon, wherein, the specific surface area of the activated carbon product is 1161m2/g、
1172m2/ g or 1259m2/g。
The method that the self-activation method prepares activated carbon, wherein, the yield of the activated carbon product is more than 17%.
The method that the self-activation method prepares activated carbon, wherein, the default chilling temperature is less than 100 DEG C.
The method that the self-activation method prepares activated carbon, wherein, the cooling atmosphere for carrying out the cooling treatment is nitrogen.
Self-activation method proposed by the present invention prepares the method for activated carbon in preparation process without the need for chemical reagent, without entering
Row post processing, step are relatively simple, improve the preparation quality and production efficiency of activated carbon, reduce being prepared into for activated carbon
This, has a good application prospect.
Description of the drawings
Fig. 1 is the nitrogen that the self-activation method that first embodiment of the invention is proposed prepares activated carbon product in the method for activated carbon
Adsorption isotherm；
Fig. 2 is the aperture that the self-activation method that first embodiment of the invention is proposed prepares activated carbon product in the method for activated carbon
Distribution map；
Fig. 3 is the nitrogen that the self-activation method that second embodiment of the invention is proposed prepares activated carbon product in the method for activated carbon
Adsorption isotherm；
Fig. 4 is the aperture that the self-activation method that second embodiment of the invention is proposed prepares activated carbon product in the method for activated carbon
Distribution map；
Fig. 5 is the nitrogen that the self-activation method that third embodiment of the invention is proposed prepares activated carbon product in the method for activated carbon
Adsorption isotherm；
Fig. 6 is the aperture that the self-activation method that third embodiment of the invention is proposed prepares activated carbon product in the method for activated carbon
Distribution map.
Specific embodiment
For the ease of understanding the present invention, the present invention is described more fully below with reference to relevant drawings.In accompanying drawing
Give the first-selected embodiment of the present invention.But, the present invention can be realized in many different forms, however it is not limited to this paper institutes
The embodiment of description.On the contrary, the purpose for providing these embodiments is to make to the disclosure more thoroughly comprehensively.
Unless otherwise defined, all of technology used herein and scientific terminology and the technical field for belonging to the present invention
The implication that technical staff is generally understood that is identical.The term for being used in the description of the invention herein is intended merely to description tool
The purpose of the embodiment of body, it is not intended that of the invention in limiting.Term as used herein " and/or " including one or more phases
The arbitrary and all of combination of the Listed Items of pass.
The present invention proposes a kind of method that self-activation method prepares activated carbon, and concrete steps include：
Biological raw material is carried out into the pretreated feedstock that pulverization process obtains 60-300 mesh.Wherein, the biological raw material includes
Stalk, bagasse and peanut shell.The pre- of composite demand is obtained after the biological raw material is carried out fully crushing in pulverizer
Fully it is dried in the environment of 105 DEG C after processing raw material again, to be dried finishing treats that next step is processed afterwards.
Pretreated feedstock Jing temperature programmings are simultaneously warming up to 800-1200 DEG C with the heating rate of 10-100 DEG C/min
After activation temperature, then intermediate product is obtained after carrying out activation process 5-10h.By the pretreatment of process abundant dried process
Raw material carries out temperature programming process in high temperature furnace, according to the different heating rate (10- of the different choice of the pretreated feedstock
100 DEG C/min) hyperthermic treatment is carried out, carry out after certain temperature range (800-1200 DEG C) is warming up to during activation process obtains
Between product.
The intermediate product is carried out cooling treatment to take out to default chilling temperature, that is, is obtained specific surface area and is more than
1100m2The activated carbon product of/g.Wherein, as the temperature of the intermediate product for obtaining is still higher, need to carry out at cooling
Reason.It is general, cooling treatment is carried out in nitrogen atmosphere to the intermediate product and obtains temperature and further taken out less than 100 DEG C afterwards obtaining final product
To activated carbon product.
Embodiment 1
A certain amount of stalk is chosen first, stalk is fully crushed to into 60 mesh in pulverizer, after then crushing
Stalk pretreated straw powder is fully dried to obtain under 105 DEG C of environment temperature；
The above-mentioned pretreated straw powder after abundant dried process of 50g is weighed after the completion of to be dried, in adding high temperature furnace
Activation process is ready for, and in the present embodiment, 950 DEG C is warming up to the heating rate of 50 DEG C/min and stable in the temperature,
Activated carbon intermediate product is obtained after activation 3h；
The activated carbon intermediate product after activation is cooled to less than 100 DEG C to then take out in nitrogen atmosphere,
Specific surface area is obtained for 1161m2The activated carbon product of/g.
Refer to Fig. 1, Fig. 1 is that the self-activation method that first embodiment of the invention is proposed prepares activated carbon in the method for activated carbon
The nitrogen adsorption isotherm of product, it will be seen from figure 1 that obtained activated carbon product relative pressure range be 0-0.2 it
Between adsorbance abruptly increase to nitrogen, when relative pressure range is between 0.2-0.8, adsorbance of the activated carbon product to nitrogen
A plateau value is reached, has illustrated absorption now already close to saturation.Can sentence with reference to the value of relative pressure and adsorbance
It is disconnected：Activated carbon product obtained by first embodiment of the invention possesses the microcellular structure of prosperity, with good absorption property.Please
Refering to Fig. 2, Fig. 2 is the aperture that the self-activation method that first embodiment of the invention is proposed prepares activated carbon product in the method for activated carbon
Distribution map, figure it is seen that the aperture of obtained activated carbon product is mainly distributed near 4nm, the work of the pore size
Property charcoal product has excellent adsorption capacity.Additionally, table 1 is the yield of the activated carbon product obtained by different embodiments, compares table
The related data of area and iodine sorption value, with reference to table 1 it is known that in the present embodiment, the yield of activated carbon product is
17.3%, iodine sorption value is 1081.9mg/g.
Embodiment 2
A certain amount of bagasse is chosen first, bagasse is fully crushed to into 80 mesh in pulverizer, then by powder
Bagasse after broken is fully dried to obtain pretreatment cane powder under 105 DEG C of environment temperature；
The above-mentioned pretreatment cane powders after abundant dried process of 50g are weighed after the completion of to be dried, in adding high temperature furnace
Activation process is ready for, and in the present embodiment, 900 DEG C is warming up to the heating rate of 30 DEG C/min and stable in the temperature,
Activated carbon intermediate product is obtained after activation 4h；
The activated carbon intermediate product after activation is cooled to less than 100 DEG C to then take out in nitrogen atmosphere,
Specific surface area is 1259m2The activated carbon product of/g.
Refer to Fig. 3, Fig. 3 is that the self-activation method that second embodiment of the invention is proposed prepares activated carbon in the method for activated carbon
The nitrogen adsorption isotherm of product, from figure 3, it can be seen that obtained activated carbon product relative pressure range be 0-0.2 it
Between adsorbance abruptly increase to nitrogen, when relative pressure range is between 0.2-0.8, adsorbance of the activated carbon product to nitrogen
A plateau value is reached, has illustrated absorption now already close to saturation.Can sentence with reference to the value of relative pressure and adsorbance
It is disconnected：Activated carbon product obtained by second embodiment of the invention possesses the microcellular structure of prosperity, with very excellent adsorptivity
Energy.At the same time, refer to Fig. 4, it is living in the method for activated carbon that Fig. 4 is prepared by the self-activation method that second embodiment of the invention is proposed
The graph of pore diameter distribution of property charcoal product, from fig. 4, it can be seen that the aperture of obtained activated carbon product is mainly distributed near 4nm,
Illustrate that using this kind of activated carbon product prepared by bagasse be microporous activated carbon, the activated carbon product of the pore size has excellent
Adsorption capacity.With reference to table 1 it is known that in the present embodiment, the yield of activated carbon product is 18.5%, illustrates to utilize sugarcane
Slag come prepare activated carbon for stalk and peanut shell have of a relatively high yield.Additionally, iodine sorption value is
1126.8mg/g, the iodine sorption value of the activated carbon product obtained by the present embodiment is relative to obtained in two other embodiment
The iodine sorption value of activated carbon product is big, and the quantity in the aperture for illustrating to be distributed in 1.0nm or so is relatively more.
Embodiment 3
A certain amount of peanut shell is chosen first, peanut shell is fully crushed to into 100 mesh in pulverizer, then by powder
Bagasse after broken is fully dried to obtain pretreatment peanut shell powder under 105 DEG C of environment temperature；
The above-mentioned pretreatment cane powders after abundant dried process of 50g are weighed after the completion of to be dried, in adding high temperature furnace
Activation process is ready for, and in the present embodiment, 1000 DEG C is warming up to the heating rate of 30 DEG C/min and stable in the temperature,
Activated carbon intermediate product is obtained after activation 2.5h；
The activated carbon intermediate product after activation is cooled to less than 100 DEG C to then take out in nitrogen atmosphere,
Specific surface area is 1172m2The activated carbon product of/g.
Refer to Fig. 5, Fig. 5 is that the self-activation method that third embodiment of the invention is proposed prepares activated carbon in the method for activated carbon
The nitrogen adsorption isotherm of product, from fig. 5, it can be seen that obtained activated carbon product relative pressure range be 0-0.2 it
Between adsorbance abruptly increase to nitrogen, when relative pressure range is between 0.2-0.8, adsorbance of the activated carbon product to nitrogen
Reached a plateau value, illustrated absorption now already close to saturation, the adsorption tendency and above-mentioned first embodiment and on
The adsorption tendency for stating second embodiment is identical.Additionally, the size with reference to relative pressure and adsorbance may determine that：The present invention the
Three embodiments possess the microcellular structure of prosperity using the activated carbon product obtained by peanut shell, with very excellent adsorptivity
Energy.At the same time, refer to Fig. 6, it is living in the method for activated carbon that Fig. 6 is prepared by the self-activation method that third embodiment of the invention is proposed
The graph of pore diameter distribution of property charcoal product, from fig. 6, it can be seen that the aperture of obtained activated carbon product is mainly distributed near 3nm,
Illustrate that using this kind of activated carbon product prepared by bagasse be microporous activated carbon, the activated carbon product of the pore size has excellent
Adsorption capacity.Additionally, combining table 1 it is known that in the present embodiment, the yield of activated carbon product is 17.7%, iodine absorption
It is worth for 1077.5mg/g.
Table 1
| Yield (%) | Specific surface area (m2/g) | Iodine sorption value (mg/g) | |
| Embodiment 1 | 17.3 | 1161 | 1081.9 |
| Embodiment 2 | 18.5 | 1259 | 1126.8 |
| Embodiment 3 | 17.7 | 1172 | 1077.5 |
In sum, comparative example 1 to 3 is it is known that produced using the activated carbon obtained by bagasse in example 2
The yield of product is maximum, and corresponding specific surface area and iodine sorption value are also maximum.Illustrate the activated carbon prepared using bagasse
Product has more excellent adsorption activity.
Self-activation method proposed by the present invention prepares the method for activated carbon in preparation process without the need for chemical reagent, without entering
Row post processing, step are relatively simple, improve the preparation quality and production efficiency of activated carbon, reduce being prepared into for activated carbon
This, has a good application prospect.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more concrete and detailed, but and
Therefore the restriction to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, without departing from the inventive concept of the premise, some deformations and improvement can also be made, these belong to the guarantor of the present invention
Shield scope.Therefore, the protection domain of patent of the present invention should be defined by claims.
Claims (10)
1. a kind of method that self-activation method prepares activated carbon, it is characterised in that comprise the following steps：
Biological raw material is carried out into the pretreated feedstock that pulverization process obtains 60-300 mesh；
Pretreated feedstock Jing temperature programmings are simultaneously warming up to 800-1200 DEG C of activation with the heating rate of 10-100 DEG C/min
After temperature, then intermediate product is obtained after carrying out activation process 5-10h；
The intermediate product is carried out cooling treatment to take out to default chilling temperature, that is, specific surface area is obtained more than 1100m2/g
Activated carbon product.
2. the method that self-activation method according to claim 1 prepares activated carbon, it is characterised in that the biological raw material is straw
Stalk, bagasse or peanut shell.
3. the method that self-activation method according to claim 1 prepares activated carbon, it is characterised in that the pretreated feedstock
Particle size is 60 mesh, 80 mesh or 100 mesh.
4. the method that self-activation method according to claim 1 prepares activated carbon, it is characterised in that the heating rate is 30
DEG C/min or 50 DEG C/min.
5. the method that self-activation method according to claim 1 prepares activated carbon, it is characterised in that the activation temperature is
900 DEG C, 950 DEG C or 1000 DEG C.
6. the method that self-activation method according to claim 1 prepares activated carbon, it is characterised in that carry out the activation process
Time be 2.5h, 3h or 4h.
7. the method that self-activation method according to claim 1 prepares activated carbon, it is characterised in that the activated carbon product
Specific surface area is 1161m2/g、1172m2/ g or 1259m2/g。
8. the method that self-activation method according to claim 1 prepares activated carbon, it is characterised in that the activated carbon product
Yield is more than 17%.
9. the method that self-activation method according to claim 1 prepares activated carbon, it is characterised in that the default chilling temperature
Less than 100 DEG C.
10. the method that self-activation method according to claim 1 prepares activated carbon, it is characterised in that carry out at the cooling
The cooling atmosphere of reason is nitrogen.
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Cited By (2)
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| CN107555430A (en) * | 2017-09-01 | 2018-01-09 | 中国林业科学研究院林产化学工业研究所 | A kind of ultracapacitor pine needle matrix activated carbon and one step charing preparation method |
| CN109019595A (en) * | 2018-09-29 | 2018-12-18 | 中国林业科学研究院林产化学工业研究所 | The method that the one step pyrolysis of biomass low pressure prepares high performance active carbon in tube furnace |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107555430A (en) * | 2017-09-01 | 2018-01-09 | 中国林业科学研究院林产化学工业研究所 | A kind of ultracapacitor pine needle matrix activated carbon and one step charing preparation method |
| CN107555430B (en) * | 2017-09-01 | 2020-05-29 | 中国林业科学研究院林产化学工业研究所 | Pine needle-based activated carbon for supercapacitor and one-step carbonization preparation method thereof |
| CN109019595A (en) * | 2018-09-29 | 2018-12-18 | 中国林业科学研究院林产化学工业研究所 | The method that the one step pyrolysis of biomass low pressure prepares high performance active carbon in tube furnace |
| CN109019595B (en) * | 2018-09-29 | 2021-11-30 | 中国林业科学研究院林产化学工业研究所 | Method for preparing high-performance activated carbon by biomass low-pressure one-step pyrolysis in tubular furnace |
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