CN106744951A - A kind of quick method for preparing activated carbon - Google Patents
A kind of quick method for preparing activated carbon Download PDFInfo
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- CN106744951A CN106744951A CN201710172549.2A CN201710172549A CN106744951A CN 106744951 A CN106744951 A CN 106744951A CN 201710172549 A CN201710172549 A CN 201710172549A CN 106744951 A CN106744951 A CN 106744951A
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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
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
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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
- C01P2006/40—Electric properties
Abstract
The present invention is to provide a kind of quick method for preparing activated carbon.Activated carbon raw material are broken into powder by step one;Step 2, is 1 according to mass ratio by activated carbon raw material powder and molten low melting point salt:1~80 ratio is uniformly mixed;Step 3, mixture is inserted in glass container, in household microwave oven under microwave action carbonization-activation 1~15 minute, microwave frequency is 2450MHz, and power is 1000W, after reaction terminates, is cooled to room temperature and activated carbon intermediate product is obtained;Step 4, by activated carbon intermediate product salt acid elution, then is washed with deionized to neutrality, and 120 DEG C of dryings obtain activated carbon to constant weight.The present invention is easy to operate, and equipment is simple, and household microwave oven, the reaction time is short, energy saving, environmental protection.The activated carbon of preparation has abundant pore structure, and pore-size distribution is moderate, and specific surface area is 1000m2·g‑1~3500m2·g‑1。
Description
Technical field
The present invention relates to a kind of method for preparation of active carbon.
Background technology
Activated carbon is a kind of porous carbon material, is, by the porous solid matter of the black of activation process, to be sent out with height
The pore structure for reaching and big specific surface area, and its stable chemical nature, the features such as with acidproof, alkaline-resisting, high temperature resistant, do not dissolve in
Water and organic solvent, oneself is widely used in the fields such as chemical industry, food processing, transportation and energy, health care, agricultural.
The method for preparing activated carbon mainly includes physical activation method, chemical activation method.Physical activation method is usually using dioxy
Change the atmosphere such as carbon or water vapour, treatment temperature is 600-1200 DEG C.Its process characteristic is:Activation temperature is high, the time is long, energy consumption
It is high.Compared with physical activation method, chemical activation method activating treatment temperature decreases in 400~900 DEG C of temperature, temperature, the time
Shorten.But both the above method is required for completing at a higher temperature, and the reaction time is long, therefore energy consumption is restriction
The major issue of its development, and its requirement to equipment is high, and cost is high, simultaneously because the waste water produced in production process and useless
If it is larger that gas deals with environmental pollution improperly, therefore can not be widely applied industrially, need to further research and solve.
At present, microwave technology has turned into substantial amounts of mature technology in national economy, in the research of function new material,
Obtain increasingly extensive application.Heating using microwave belongs to " radiation " heating.Can be by the dielectric loss of heating object confrontation microwave
And realize " penetration " heating of body phase, simultaneously because not heating environment medium, is in the very short time (even moment)
Can reach hundreds if not thousands of high temperature so that it is high, quick etc. excellent without thermal inertia, energy-conservation that heating using microwave shows the efficiency of heating surface
Point, can easily realize being rapidly heated, or high frequency time large-scale production.Such as patent of the A of Publication No. CN 102502611
Disclose a kind of using vacuum microwave heating, the method that rapid, high volume prepares Graphene in file;Publication No. CN
A kind of method for preparing activated carbon as raw material microwave method with waste leather is disclosed in the patent document of 103145126 A.But more than
Method in patent document is required for completing in a vacuum or inert atmosphere, especially the former, the equipment of reaction is industrial microwave
Stove is, it is necessary to vacuum microwave is heated, therefore working condition is the major issue for restricting its development.
The content of the invention
It is easy to operate it is an object of the invention to provide one kind, the reaction time short quick method for preparing activated carbon.
The object of the present invention is achieved like this:
Activated carbon raw material are broken into powder by step one;
Step 2, is 1 according to mass ratio by activated carbon raw material powder and molten low melting point salt:1~80 ratio is carried out
Uniform mixing;
Step 3, mixture is inserted in glass container, in household microwave oven under microwave action carbonization-activation 1~15
Minute, microwave frequency is 2450MHz, and power is 1000W, after reaction terminates, is cooled to room temperature and activated carbon intermediate product is obtained;
Step 4, by activated carbon intermediate product salt acid elution, then is washed with deionized to neutrality, and 120 DEG C of dryings are extremely
Constant weight, obtains activated carbon.
The present invention can also include:
1st, the activated carbon raw material are coal, coconut husk, stalk, bean curd powder, rice hulls, wood chip, marine alga or glucose.
2nd, the molten low melting point salt is ZnCl2, KCl and ZnCl2Molal weight than the mixture for 48/52, KOH with
Molal weight of the molal weight of NaOH than the mixture for 49/51, KI and LiI is than the mixture for 37/63.
For the defect in prior art, the present invention is provided for the problem of high energy consumption and working condition in prior art
A kind of method that fuse salt assisted microwave synthesis method prepares activated carbon, the method is easy to operate, and equipment is simple, and household microwave oven is
Can, the reaction time is short, energy saving, environmental protection.
Ultracapacitor can be applied to using the activated carbon obtained by the method for the present invention, lithium ion battery, fuel cell,
Adsorbent, catalyst carrier, natural gas, storage of hydrogen etc..
Compared with prior art, the present invention has following beneficial effect:
(1) present invention is by the use of low temperature molten salt as activator, using household microwave oven as carbonizing apparatus.Low-temperature molten salt exists
The contact of the carbon with air of generation can be avoided in carbonisation, therefore does not need vacuum or extra inert gas shielding, letter
Experimental provision and equipment requirement are changed.Secondly fuse salt can be as template during carbonization, and it is close during the course of the reaction
It is distributed between carbon particle, hinders the interconnection between particle, such that it is able to regulates and controls the pore structure of carbon material.Therefore this hair
The activated carbon of bright preparation has abundant pore structure, and pore-size distribution is moderate, and specific surface area is 1000m2·g-1~3500m2·g-1,
The application of the aspects such as the storage of ultracapacitor, adsorbent, catalyst carrier and natural gas, hydrogen can be fully met.
(2) the method is easy to operate, and equipment is simple, only needs household microwave oven, and process is simple and quick, the reaction time
Short, energy saving is a kind of simple and feasible practical approach, and can realize prepared by scale magnanimity.Microwave belongs to body phase
Penetration is heated, and accumulation form, modes of emplacement with sample etc. are unrelated.The cavity of micro-wave oven is bigger, and the presoma that can be put into is just
More, the activated carbon for obtaining is more, it is adaptable to industrialized production prepared by activated carbon.
Brief description of the drawings
Fig. 1:The SEM figures of the activated carbon that embodiment 1 is obtained.
Fig. 2:The XRD of the activated carbon that embodiment 1 is obtained.
Fig. 3:The N of the activated carbon that embodiment 1 is obtained2Adsorption/desorption figure.
Fig. 4:Specific capacitance value of the activated carbon that embodiment 1 is obtained under different discharge current densities.
Specific embodiment
The present invention is described in detail for citing below.It is further that following examples will be helpful to those skilled in the art
Understand the present invention, but the invention is not limited in any way.It should be pointed out that to those skilled in the art,
Without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to protection model of the invention
Enclose.
Embodiment 1, ZnCl2Low temperature molten salt is used as activator, the preparation of activated carbon:
Weigh the bean curd powder (freeze-drying is obtained) of 0.25g, the ZnCl with 5g2Salt it is well mixed after, by mixture
Insert in glass beaker, move it in micro-wave oven, carbonization-activation 2 minutes under microwave action, microwave frequency is 2450MHz,
Power is 1000W, after reaction terminates, is taken out after being cooled to room temperature, activated carbon intermediate product is obtained, in the middle of obtained activated carbon
Product, uses hydrochloric acid washing impurity-removing, then is washed with deionized to neutrality, and 120 DEG C of dryings obtain activated carbon to constant weight.
Physics and chemistry is carried out to prepared activated carbon using SEM, X-ray diffraction, the analysis of nitrogen adsorption desorption
Matter is characterized, and as a result sees Fig. 1, Fig. 2 and Fig. 3, and performance of the supercapacitor test is carried out to prepared absorbent charcoal material, as a result sees figure
4。
Fig. 1 shows that prepared absorbent charcoal material is sheet, and Fig. 2 shows, prepared activated carbon occurs two clearly
Diffraction maximum, correspondence carbon material impalpable structure.N2Adsorption/desorption curve is as shown in figure 3, activated carbon specific surface area is
1459m2·g-1.Performance of the supercapacitor test is carried out to absorbent charcoal material, such as Fig. 4 shows, 1Ag-1Under discharge current density,
Specific capacity is 380Fg-1, 50Ag-1When electric capacity be maintained as 200Fg-1。
Embodiment 2, KCl/ZnCl2Low temperature molten salt is used as activator, the preparation of activated carbon:
Weigh the bean curd powder (freeze-drying is obtained) of 0.25g, the KCl/ZnCl with 5g2(KCl and ZnCl2Molal weight
After being well mixed for salt 48/52), mixture is inserted in glass beaker, moved it in micro-wave oven, under microwave action
Carbonization-activation 2 minutes, microwave frequency is 2450MHz, and power is 1000W, after reaction terminates, is taken out after being cooled to room temperature, is obtained
Activated carbon intermediate product, by obtained activated carbon intermediate product, uses hydrochloric acid washing impurity-removing, then is washed with deionized to neutrality,
120 DEG C of dryings obtain activated carbon to constant weight.
Activated carbon specific surface area is 1280m2·g-1, absorption test is carried out to organic dyestuff magenta, when fuchsin solution concentration
It is 10mgL-1, after 24h, activated carbon is adsorbed completely substantially to it.
Embodiment 3, KOH/NaOH low temperature molten salts are used as activator, the preparation of activated carbon:
The bean curd powder (freeze-drying is obtained) of 0.25g is weighed, the KOH/NaOH (molal weights of KOH and NaOH with 5g
After being well mixed for salt 49/51), mixture is inserted in glass beaker, moved it in micro-wave oven, under microwave action
Carbonization-activation 2 minutes, microwave frequency is 2450MHz, and power is 1000W, after reaction terminates, is taken out after being cooled to room temperature, is obtained
Activated carbon intermediate product, by obtained activated carbon intermediate product, uses hydrochloric acid washing impurity-removing, then is washed with deionized to neutrality,
120 DEG C of dryings obtain activated carbon to constant weight.
Activated carbon specific surface area is 1600m2·g-1, to carrying out adsorption hydrogen-storing test to it, in room temperature (25 DEG C), 2MPa
Hydrogen storage content is 5.82wt%.
Embodiment 4, KI/LiI low temperature molten salts are used as activator, the preparation of activated carbon:
The bean curd powder (freeze-drying is obtained) of 0.25g is weighed, (the molal weight ratio of KI and LiI is with the KI/LiI of 5g
37/63) after salt is well mixed, mixture is inserted in glass beaker, is moved it in micro-wave oven, carbonized under microwave action
Activation 2 minutes, microwave frequency is 2450MHz, and power is 1000W, after reaction terminates, is taken out after being cooled to room temperature, and activity is obtained
Charcoal intermediate product, by obtained activated carbon intermediate product, uses hydrochloric acid washing impurity-removing, then be washed with deionized to neutrality, 120 DEG C
Dry to constant weight, obtain activated carbon.
Activated carbon specific surface area is 1200m2·g-1, as Pt nano-particle catalyst carriers, it is tested,
It was found that Pt/C has catalysis methanol electroxidation performance high.
Claims (6)
1. a kind of quick method for preparing activated carbon, it is characterized in that:
Activated carbon raw material are broken into powder by step one;
Step 2, is 1 according to mass ratio by activated carbon raw material powder and molten low melting point salt:1~80 ratio is carried out uniformly
Mixing;
Step 3, mixture is inserted in glass container, in household microwave oven under microwave action 1~15 point of carbonization-activation
Clock, microwave frequency is 2450MHz, and power is 1000W, after reaction terminates, is cooled to room temperature and activated carbon intermediate product is obtained;
Step 4, by activated carbon intermediate product salt acid elution, then is washed with deionized to neutrality, 120 DEG C of dryings to constant weight,
Obtain activated carbon.
2. the quick method for preparing activated carbon according to claim 1, it is characterized in that:The activated carbon raw material be coal,
Coconut husk, stalk, bean curd powder, rice hulls, wood chip, marine alga or glucose.
3. the quick method for preparing activated carbon according to claim 1 and 2, it is characterized in that:The molten low melting point salt is
ZnCl2。
4. the quick method for preparing activated carbon according to claim 1 and 2, it is characterized in that:The molten low melting point salt is
KCl and ZnCl2Molal weight than the mixture for 48/52
5. the quick method for preparing activated carbon according to claim 1 and 2, it is characterized in that:The molten low melting point salt is
The molal weight of KOH and NaOH is than the mixture for 49/51.
6. the quick method for preparing activated carbon according to claim 1 and 2, it is characterized in that:The molten low melting point salt is
The molal weight of KI and LiI is than the mixture for 37/63.
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Cited By (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107021484A (en) * | 2017-06-19 | 2017-08-08 | 江苏竹溪活性炭有限公司 | Water purification activated carbon |
CN107376940A (en) * | 2017-07-31 | 2017-11-24 | 江苏金环环保设备有限公司 | A kind of catalytic composite material of rapidly and efficiently renovation of organic pollution soil and preparation method thereof |
CN107399730A (en) * | 2017-08-22 | 2017-11-28 | 河南师范大学 | The method that the carbonization of one step prepares biomass-based porous carbon materials |
CN107697914A (en) * | 2017-08-22 | 2018-02-16 | 河南师范大学 | A kind of method for preparing nitrogen-doped porous carbon material |
CN108083276A (en) * | 2017-12-29 | 2018-05-29 | 北海星石碳材料科技有限责任公司 | The preparation method of ultracapacitor activated carbon |
CN108217646A (en) * | 2018-01-05 | 2018-06-29 | 珠海市吉林大学无机合成与制备化学重点实验室 | A kind of preparation method of porous Si-C composite material |
CN108394889A (en) * | 2018-05-22 | 2018-08-14 | 东北大学 | A kind of method and apparatus extracting carbon material from plastics |
CN109160514A (en) * | 2018-09-21 | 2019-01-08 | 四川理工学院 | A kind of bean curd expanding method and the classifying porous active carbon of preparation method and bean curd of soybean flour and preparation method thereof |
CN109161915A (en) * | 2018-09-30 | 2019-01-08 | 东北大学 | The method for preparing activated carbon for super capacitors powder using coal based on fused salt |
CN109437194A (en) * | 2019-01-04 | 2019-03-08 | 新疆大学 | The method that one step molte-salt synthesis prepares coal base porous charcoal Yu metal oxide nano hybrid material |
CN109865508A (en) * | 2019-04-09 | 2019-06-11 | 福建农林大学 | A kind of method of ultrasonic wave added melting eutectic alkali regenerating waste active carbon |
CN111321428A (en) * | 2020-03-04 | 2020-06-23 | 中南大学 | Method for waste mercuric chloride catalyst molten salt electrolysis regeneration and mercury recovery |
CN113036102A (en) * | 2021-03-04 | 2021-06-25 | 哈尔滨工程大学 | Molybdenum selenide composite carbonized common sowthistle herb flower crown hair electrode material for sodium ion battery |
CN117550600A (en) * | 2024-01-11 | 2024-02-13 | 河南科技学院 | Porous biomass carbon electrode material, preparation method of electrode slice of porous biomass carbon electrode material and electrode slice |
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Cited By (16)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107021484A (en) * | 2017-06-19 | 2017-08-08 | 江苏竹溪活性炭有限公司 | Water purification activated carbon |
CN107376940A (en) * | 2017-07-31 | 2017-11-24 | 江苏金环环保设备有限公司 | A kind of catalytic composite material of rapidly and efficiently renovation of organic pollution soil and preparation method thereof |
CN107399730A (en) * | 2017-08-22 | 2017-11-28 | 河南师范大学 | The method that the carbonization of one step prepares biomass-based porous carbon materials |
CN107697914A (en) * | 2017-08-22 | 2018-02-16 | 河南师范大学 | A kind of method for preparing nitrogen-doped porous carbon material |
CN108083276B (en) * | 2017-12-29 | 2020-12-01 | 北海星石碳材料科技有限责任公司 | Preparation method of super capacitor activated carbon |
CN108083276A (en) * | 2017-12-29 | 2018-05-29 | 北海星石碳材料科技有限责任公司 | The preparation method of ultracapacitor activated carbon |
CN108217646A (en) * | 2018-01-05 | 2018-06-29 | 珠海市吉林大学无机合成与制备化学重点实验室 | A kind of preparation method of porous Si-C composite material |
CN108394889A (en) * | 2018-05-22 | 2018-08-14 | 东北大学 | A kind of method and apparatus extracting carbon material from plastics |
CN108394889B (en) * | 2018-05-22 | 2022-05-27 | 东北大学 | Method and equipment for extracting carbon material from plastic |
CN109160514A (en) * | 2018-09-21 | 2019-01-08 | 四川理工学院 | A kind of bean curd expanding method and the classifying porous active carbon of preparation method and bean curd of soybean flour and preparation method thereof |
CN109161915A (en) * | 2018-09-30 | 2019-01-08 | 东北大学 | The method for preparing activated carbon for super capacitors powder using coal based on fused salt |
CN109437194A (en) * | 2019-01-04 | 2019-03-08 | 新疆大学 | The method that one step molte-salt synthesis prepares coal base porous charcoal Yu metal oxide nano hybrid material |
CN109865508A (en) * | 2019-04-09 | 2019-06-11 | 福建农林大学 | A kind of method of ultrasonic wave added melting eutectic alkali regenerating waste active carbon |
CN111321428A (en) * | 2020-03-04 | 2020-06-23 | 中南大学 | Method for waste mercuric chloride catalyst molten salt electrolysis regeneration and mercury recovery |
CN113036102A (en) * | 2021-03-04 | 2021-06-25 | 哈尔滨工程大学 | Molybdenum selenide composite carbonized common sowthistle herb flower crown hair electrode material for sodium ion battery |
CN117550600A (en) * | 2024-01-11 | 2024-02-13 | 河南科技学院 | Porous biomass carbon electrode material, preparation method of electrode slice of porous biomass carbon electrode material and electrode slice |
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