CN110127694A - A kind of preparation method of asphalt based active carbon - Google Patents
A kind of preparation method of asphalt based active carbon Download PDFInfo
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- CN110127694A CN110127694A CN201910414167.5A CN201910414167A CN110127694A CN 110127694 A CN110127694 A CN 110127694A CN 201910414167 A CN201910414167 A CN 201910414167A CN 110127694 A CN110127694 A CN 110127694A
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- Prior art keywords
- active carbon
- preparation
- coal tar
- method described
- tar pitch
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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
- C01B32/33—Preparation characterised by the starting materials from distillation residues of coal or petroleum; from petroleum acid sludge
-
- 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
The invention discloses a kind of preparation methods of asphalt based active carbon, and coal tar pitch and other carbonaceous materials are made high-intensitive low-resistance active carbon after broken, homogenizing, kneading, die mould, activation, broken, washing drying and other steps.Compared with traditional preparation methods, this method can be evenly dispersed by activator and be fixed in other materials, the preferable active carbon of pore-size distribution is capable of forming by in-situ activation, with biggish stability, the utilization efficiency of alkali in process for preparing active carbon greatly improved, reduce and container corrosion and impurity element are brought into, and since there is no limit can greatly improve the preparation efficiency of active carbon to the heating rate to activation process.The intensity with higher of active carbon prepared by this method and preferable electric conductivity, tap density reach 0.53-0.65g/cm3, resistivity reached 65-80 μ Ω m.
Description
Technical field
The present invention relates to porous carbon material preparation fields, and in particular to a kind of method of porous carbon material preparation.
Background technique
Active carbon is a kind of Carbon Materials with class graphite microcrystalline structure, is the production obtained after certain activating process
Object.It is typically represented as porous carbon material, due to huge specific surface area, porous structure and stronger adsorption capacity
The features such as, it is widely used in the new energy fields such as lithium cell negative pole material, supercapacitor.And in these fields for active carbon
There is higher requirement: biggish specific surface area, suitable pore-size distribution, quantity of suitable surface functional group etc..And coal drips
Green one kind as the numerous raw materials for preparing active carbon, has many advantages, such as that ash content is low, carbonization yield is high, source is wide, has received
Extensive concern.
Using the high performance active carbon that coal tar pitch is prepared as raw material, there are more patent and documents.Wherein
CN103803550A, CN 105174260A are laid particular emphasis on using coal tar pitch as raw material by the coking of pitch elder generation, then through broken and activation
Agent is mixed, and direct after mixing or increase pre-activate process, the asphalt based active carbon of preparation is used for supercapacitor.It is above-mentioned special
Benefit still biases toward traditional handicraft, proposes requirement to heating rate, entire production technology is difficult to keep stable, and gained
Active carbon electric conductivity and intensity are lower.In addition also utilization efficiency not of the invention is high for the utilization rate of the alkali of above-mentioned patent.And
Asphalt production process is used involved by patent CN106904612A, first by asphalt modulation at the pitch of high softening-point, then is passed through
Active carbon is made in crushing molding, charing, activation.The method of the active carbon of the patent have the characteristics that it is complicated for operation, but also need
To be carbonized and be activated two steps realize active carbon prepare, cause biggish energy waste, and to heating rate it is also proposed that
Detailed requirement, is more likely to the preparation of column-shaped active carbon.
The preparation method of the active carbon of new energy field according to the present invention can be good at solving above-mentioned problem, together
There is no pertinent literatures in terms of Shi Tigao asphalt based active carbon intensity and electric conductivity.
Summary of the invention
Aiming at the shortcomings of the prior art, the present invention provides a kind of preparation method of asphalt based active carbon.Simultaneous interpretation
Controlling Preparation Method is compared, and this method can be evenly dispersed by activator and be fixed in other materials, can by in-situ activation
The preferable active carbon of pore-size distribution is formed, there is biggish stability, the utilization of alkali in process for preparing active carbon greatly improved
Efficiency reduces and brings into container corrosion and impurity element, and since there is no limit energy for the heating rate to activation process
Enough greatly improve the preparation efficiency of active carbon.This method is achieved through the following technical solutions:
1) coal tar pitch and other Carbon Materials are subjected to broken sieving processing；
2) coal tar pitch, other Carbon Materials and activator are homogenized processing；
3) binder is added in mixture after handling, and carries out kneading processing；
4) mixture after kneading carries out die mould；
5) mixture after die mould is activated；
6) material after activation is crushed, is washed.
Further, break process is carried out to coal tar pitch in step (1), granularity controls below -80 mesh.
Further, break process is carried out to other Carbon Materials in step (1), granularity controls below -100 mesh.
Further, other materials used in step (1) is petroleum coke, calcined coke, pitch coke, natural graphite, artificial graphite
A kind of or several combination.
Further, step (2) is coal tar pitch, other Carbon Materials, KOH that will be handled in step (1) etc. using batch mixer
Mixing processing is carried out, incorporation time is controlled in 2min-60min.
Further, the binder that step (2) is added is to can be cellulose, sodium carboxymethylcellulose, polyvinyl alcohol, shallow lake
Powder, lignin adhesive, pyrolysis bio-oils adhesive, coal tar etc..
Further, the binder content that step (2) is added accounts for coal tar pitch and other Carbon Materials gross mass ratios are
0.5%-30%.
Further, the quality of the other materials such as petroleum coke, calcined coke, pitch coke, natural graphite, artificial graphite and pitch
Than for 0.2:10-1:10.
Further, the mixture handled in step (3) is pressed and molded by step (4), and briquetting pressure control exists
0.1Mpa-100MPa。
Further, step (5) be by the raw material after step (4) medium-pressure type under an inert atmosphere or land-fill method is lived
Change processing is activated heating rate and selects 4 DEG C/min, can also select other heating rates.
Further, 650-900 DEG C of activation temperature in step (5), soaking time 2-3h.
Further, the sample after step (5) activation is carried out break process by step (6), and treated, and sample is dissolved into
In deionized water, being neutralized with hydrochloric acid to PH is 6-7, and controls 25-70 DEG C of temperature, stirs 2-10h.
Further, the sample that step (6) are handled is filtered, the sample after suction filtration is dried at 110 DEG C, is dried
The dry time is 3-8h.
Further, sample broke in step (5) is sieved, Control granularity is in 200 mesh hereinafter, the activity prepared
Charcoal.
Advantageous effects of the invention:
1) this technique has biggish stability, and the utilization efficiency of alkali in process for preparing active carbon greatly improved.
2) activator is stirred with raw material by binder at normal temperature by this method, being formed has the mixed of certain plasticity
Close material, at the same by molding mode by activator it is evenly dispersed and it is fixed in the feed, aperture is capable of forming by in-situ activation
It is distributed preferable active carbon.
3) the method reduce the contact in process for preparing active carbon with container, reduce to container corrosion and impurity element
Bring into, and due to the heating rate to activation process there is no limit, the preparation efficiency of active carbon can be greatly improved.
4) active carbon intensity with higher and preferable electric conductivity, tap density prepared by this method reach 0.53-
0.65g/cm3, resistivity reached 65-80 μ Ω m.
Detailed description of the invention
Fig. 1 is asphalt based active carbon preparation method flow chart.
Specific embodiment
The present invention will further illustrate embodiment by the description of following embodiments, but the present invention is not intended to be limited to down
State embodiment.
Embodiment 1
It carries out coal tar pitch to be crushed to -80 mesh hereinafter, breaking calcined coke with below extremely -100 mesh.According to pitch and calcined coke
Ratio be that 10:0.2 is mixed, then with KOH be uniformly mixed and be added that binder fiber is plain, and additional amount is in mixed process
0.5%.After kneading, mixture is formed by the way of compression molding, molding parameter are as follows: pressure 0.1Mpa.It again will be at
The material of type, which is put into stove, to be activated, activating process parameter are as follows: and 600 DEG C of temperature, time 3h.The broken washing of the material activated
To neutrality, temperature is controlled to 25 DEG C, then is filtered, and 110 DEG C of drying in an oven, dry 8h after suction filtration.Gained activated carbon bodies
Product density is 0.53g/cm3, resistivity reached 80 μ Ω m.
Embodiment 2
It carries out coal tar pitch to be crushed to -80 mesh hereinafter, breaking calcined coke with below extremely -100 mesh.According to pitch and calcined coke
Ratio be that 10:0.5 is mixed, then with KOH be uniformly mixed and be added that binder fiber is plain, and additional amount is in mixed process
2%.After kneading, mixture is formed by the way of compression molding, molding parameter are as follows: pressure 10Mpa.It again will be molding
Material, which is put into stove, to be activated, activating process parameter are as follows: and 700 DEG C of temperature, time 3h.The broken washing of the material activated is into
Property, temperature is controlled to 25 DEG C, then is filtered, 110 DEG C of drying in an oven after suction filtration, dries 8h.Gained active carbon volume is close
Degree is 0.56g/cm3, resistivity reached 77 μ Ω m.
Embodiment 3
It carries out coal tar pitch to be crushed to -80 mesh hereinafter, breaking calcined coke with below extremely -100 mesh.According to pitch and calcined coke
Ratio be that 10:0.6 is mixed, then with KOH be uniformly mixed and be added that binder fiber is plain, and additional amount is in mixed process
8%.After kneading, mixture is formed by the way of compression molding, molding parameter are as follows: pressure 46Mpa.It again will be molding
Material, which is put into stove, to be activated, activating process parameter are as follows: and 800 DEG C of temperature, time 3h.The broken washing of the material activated is into
Property, temperature is controlled to 25 DEG C, then is filtered, 110 DEG C of drying in an oven after suction filtration, dries 8h.Gained active carbon volume is close
Degree is 0.65g/cm3, resistivity reached 65 μ Ω m.
Embodiment 4
It carries out coal tar pitch to be crushed to -80 mesh hereinafter, calcined coke is crushed to -100 mesh or less.According to pitch and calcined coke
Ratio be that 10:0.8 is mixed, then with KOH be uniformly mixed and be added that binder fiber is plain, and additional amount is in mixed process
15%.After kneading, mixture is formed by the way of compression molding, molding parameter are as follows: pressure 60Mpa.It again will molding
Material be put into stove and activated, activating process parameter are as follows: 600 DEG C of temperature, time 3h.The broken washing of the material activated is extremely
Neutrality, temperature is controlled to 25 DEG C, then is filtered, and 110 DEG C of drying in an oven, dry 8h after suction filtration.Gained active carbon volume
Density is 0.60g/cm3, resistivity reached 68 μ Ω m.
Embodiment 5
It carries out coal tar pitch to be crushed to -80 mesh hereinafter, breaking calcined coke with below extremely -100 mesh.According to pitch and calcined coke
Ratio be that 10:1 is mixed, then with KOH be uniformly mixed and be added that binder fiber is plain, and additional amount is in mixed process
20%.After kneading, mixture is formed by the way of compression molding, molding parameter are as follows: pressure 74Mpa, dwell time
3min.Molding material is put into stove again and is activated, activating process parameter are as follows: 900 DEG C of temperature, time 3h.It has activated
The broken washing of material to neutrality, temperature is controlled to 25 DEG C, then is filtered, and 110 DEG C of drying in an oven, dry 8h after suction filtration.
Gained active carbon bulk density is 0.64g/cm3, resistivity reached 67 μ Ω m.
Embodiment 6
It carries out coal tar pitch to be crushed to -80 mesh hereinafter, breaking calcined coke with below extremely -100 mesh.According to pitch and forge rear stone
The ratio of oil coke is that 10:1 is mixed, then be uniformly mixed with KOH and binder fiber element, additional amount are added in mixed process
It is 30%.After kneading, mixture is formed by the way of compression molding, molding parameter are as follows: pressure 100Mpa, when pressure maintaining
Between 3min.Molding material is put into stove again and is activated, activating process parameter are as follows: 900 DEG C of temperature, time 3h.Activation
The broken washing of complete material is to neutrality, and temperature is controlled to 25 DEG C, then is filtered, 110 DEG C of drying in an oven, drying after suction filtration
8h.Gained active carbon bulk density is 0.65g/cm3, resistivity reached 65 μ Ω m.
Embodiment 7
It carries out coal tar pitch to be crushed to -80 mesh hereinafter, breaking pitch coke with below extremely -100 mesh.According to pitch and pitch coke
Ratio be that 10:1 is mixed, then with KOH be uniformly mixed and be added that binder fiber is plain, and additional amount is in mixed process
12%.After kneading, mixture is formed by the way of compression molding, molding parameter are as follows: pressure 60Mpa.It again will molding
Material be put into stove and activated, activating process parameter are as follows: 850 DEG C of temperature, time 3h.The broken washing of the material activated is extremely
Neutrality, temperature is controlled to 25 DEG C, then is filtered, and 110 DEG C of drying in an oven, dry 8h after suction filtration.Gained active carbon volume
Density is 0.53g/cm3, resistivity reached 76 μ Ω m.
Embodiment 8
It carries out coal tar pitch to be crushed to -80 mesh hereinafter, breaking natural graphite with below extremely -100 mesh.According to pitch and naturally
The ratio of graphite is that 10:1 is mixed, then be uniformly mixed with KOH and binder fiber element, additional amount are added in mixed process
It is 12%.After kneading, mixture is formed by the way of compression molding, molding parameter are as follows: pressure 60Mpa.It again will be at
The material of type, which is put into stove, to be activated, activating process parameter are as follows: and 850 DEG C of temperature, time 3h.The broken washing of the material activated
To neutrality, temperature is controlled to 25 DEG C, then is filtered, and 110 DEG C of drying in an oven, dry 8h after suction filtration.Gained activated carbon bodies
Product density is 0.65g/cm3, resistivity reached 65 μ Ω m.
Embodiment 9
It carries out coal tar pitch to be crushed to -80 mesh hereinafter, breaking artificial graphite with below extremely -100 mesh.According to pitch with it is artificial
The ratio of graphite is that 10:1 is mixed, then be uniformly mixed with KOH and binder fiber element, additional amount are added in mixed process
It is 12%.After kneading, mixture is formed by the way of compression molding, molding parameter are as follows: pressure 60Mpa.It again will be at
The material of type, which is put into stove, to be activated, activating process parameter are as follows: and 850 DEG C of temperature, time 3h.The broken washing of the material activated
To neutrality, temperature is controlled to 25 DEG C, then is filtered, and 110 DEG C of drying in an oven, dry 8h after suction filtration.Gained activated carbon bodies
Product density is 0.62g/cm3, resistivity reached 67 μ Ω m.
Embodiment 10
It carries out coal tar pitch to be crushed to -80 mesh hereinafter, petroleum coke is crushed to -100 mesh or less.According to pitch and petroleum coke
Burnt ratio is that 10:1 is mixed, then be uniformly mixed with KOH and binder fiber element is added in mixed process, and additional amount is
12%.After kneading, mixture is formed by the way of compression molding, molding parameter are as follows: pressure 60Mpa.It again will molding
Material be put into stove and activated, activating process parameter are as follows: 850 DEG C of temperature, time 3h.The broken washing of the material activated is extremely
Neutrality, temperature is controlled to 25 DEG C, then is filtered, and 110 DEG C of drying in an oven, dry 8h after suction filtration.Gained active carbon volume
Density is 0.56g/cm3, resistivity reached 75 μ Ω m.
Above-described is only presently preferred embodiments of the present invention, not limitation invention.It should be understood that for the general of this field
For logical technical staff, under technical inspiration provided by the present invention, other equivalent improvement can also be made, this may be implemented
The purpose of invention, is regarded as protection scope of the present invention.
Claims (9)
1. a kind of preparation method of asphalt based active carbon, it is characterised in that the following steps are included:
1) coal tar pitch and other carbonaceous materials are subjected to broken sieving processing respectively；
2) coal tar pitch, other carbonaceous materials and activator are homogenized processing；
3) binder is added in mixture after handling, and carries out kneading processing；
4) mixture after kneading carries out die mould；
5) mixture after die mould is activated；
6) material after activation is crushed, is washed, active carbon is made after dry.
2. according to preparation method described in right 1, which is characterized in that other described carbonaceous materials are petroleum coke, calcined coke, pitch
One of coke, natural graphite, artificial graphite or several combination.
3. according to preparation method described in right 1, which is characterized in that coal tar pitch granularity after broken sieving is -80
Mesh, granularity is -100 mesh after the broken sieving of other carbonaceous materials.
4. according to preparation method described in right 1, which is characterized in that the mass ratio of described other carbonaceous materials and coal tar pitch is
0.2:10~1:10.
5. according to preparation method described in right 1, which is characterized in that the homogenizing processing is by coal tar pitch, other charcoal materials
Material, activator KOH carry out mixing mixing using mixing equipment.
6. according to preparation method described in right 1, which is characterized in that the binder be cellulose, sodium carboxymethylcellulose,
Polyvinyl alcohol, starch, lignin adhesive, pyrolysis bio-oils adhesive, coal tar.
7. according to preparation method described in right 1, which is characterized in that the binder content accounts for coal tar pitch and other Carbon Materials
Gross mass ratio is 0.5%-30%.
8. according to preparation method described in right 1, which is characterized in that the die mould is using mechanical or manual molding, molding
Body keeps stable shape, briquetting pressure 0.1Mpa-100MPa at normal temperature.
9. according to preparation method described in right 1, which is characterized in that 650-900 DEG C of activation temperature, soaking time 2-3h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111217369A (en) * | 2020-03-10 | 2020-06-02 | 国家能源集团宁夏煤业有限责任公司 | Benzene protection active carbon and preparation method thereof |
| CN112010303A (en) * | 2020-08-28 | 2020-12-01 | 淮北市森化碳吸附剂有限责任公司 | Method for preparing activated carbon by using novel adhesive |
| CN115196630A (en) * | 2022-06-07 | 2022-10-18 | 谢艳 | Preparation method for improving tap density of carbon electrode material for energy storage device |
| CN115532233A (en) * | 2021-06-29 | 2022-12-30 | 中国石油化工股份有限公司 | Asphaltene-based adsorption material and preparation method and application thereof |
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Cited By (5)
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| CN115532233A (en) * | 2021-06-29 | 2022-12-30 | 中国石油化工股份有限公司 | Asphaltene-based adsorption material and preparation method and application thereof |
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| CN115196630A (en) * | 2022-06-07 | 2022-10-18 | 谢艳 | Preparation method for improving tap density of carbon electrode material for energy storage device |
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Application publication date: 20190816 |