CN107973296A - A kind of large aperture activated carbon and preparation method thereof - Google Patents
A kind of large aperture activated carbon and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to activated carbon preparation field, and in particular to a kind of large aperture activated carbon and preparation method thereof, includes the following steps：Step 1, crush activated carbon raw material, and by the raw material soaking in ethanol solution, it is expanding agent that hydroxide is additionally added in the ethanol solution, and after supersonic oscillations, water washing dries to obtain Pre-Treatment of Activated charcoal；Step 2, the Pre-Treatment of Activated charcoal add surfactant and are uniformly mixed；Step 3, heat under nitrogen protection, obtains Pre-Treatment of Activated charcoal, after nitrogen is switched to the mixed gas of vapor and carbon dioxide, activation obtains large aperture activated carbon.Beneficial effect of the present invention：First, the present invention acts on carry out reaming at the same time using physics and chemical method；Secondly, it is physically activated using the progress of the mixed gas of carbon dioxide and vapor in activation process, the aperture of activated carbon has been widened under the synergistic effect of the two.
Description
Technical field
The present invention relates to activated carbon preparation field, and in particular to a kind of large aperture activated carbon and preparation method thereof.
Background technology
Activated carbon has excellent physics and chemical stability, flourishing pore structure and high adsorption capacity, extensive
Applied to relevant industries such as food, chemical industry, environmental protection, pharmacy and new energy.Such as catalyst carrier, battery electrode, super electricity
In container, gas storage and biological medicine, it is widely applied.Wherein the activated carbon of high conductivity is in battery and super capacitor
The energy storage of device class is increasingly attracted attention with the research and development in electrode material.
Activated carbon as energy storage material, it is necessary to possess big specific surface area, because specific surface area is bigger, the appearance of activated carbon
Amount is higher, the specific capacity of energy storage material and higher than energy；Activated carbon should also have abundant macroporous structure at the same time, if hole
Footpath is too small, such as microcellular structure (r<2nm), the anion radius of solution is big, then can not spread inside micropore, causes the profit of activated carbon
Declined with rate.
The content of the invention
The technical problems to be solved by the invention are：A kind of large aperture activated carbon and preparation method thereof is provided.
The technical scheme is that providing a kind of preparation method of large aperture activated carbon, include the following steps：
Step 1, crush activated carbon raw material, by the raw material soaking in ethanol solution, is additionally added in the ethanol solution
Hydroxide is expanding agent, and after supersonic oscillations, water washing dries to obtain Pre-Treatment of Activated charcoal；
Step 2, the Pre-Treatment of Activated charcoal add surfactant and 7-9h are impregnated at a temperature of 80-100 DEG C, are spaced 2-3h
Stirring, is uniformly mixed it；
Step 3, under nitrogen protection heat 2-4 it is small when, heating-up temperature be 300-500 degree, obtains Pre-Treatment of Activated charcoal, after general
Nitrogen switches to the mixed gas of vapor and carbon dioxide, when 700-800 degree soak times 1-3 is small, obtains large aperture work
Property charcoal.
The large aperture that another technical solution of the present invention is prepared for a kind of preparation method of above-mentioned large aperture activated carbon of offer
Activated carbon.
Beneficial effect of the present invention：First, the present invention is same using physics (ultrasonic wave) and chemistry (hydroxide corrosion) method
Shi Zuoyong carries out reaming, and the molecule of liquid is subject to transmitting for the energy of ultrasonic wave, interaction of molecules and produce substantial amounts of bubble,
Bubbles burst makes activated carbon capillary crush to form mesoporous.And hydroxide dissolving is in the solution and as solution is diffused into activated carbon
Corrosiveness is played on surface, this requires that the micropore of activated carbon allows for being soaked by liquid, and immersion is more abundant, and effect is better.
Activated Carbon Pretreatment is placed in cetylpyridinium chloride solution by the present invention, Surface Groups of Active Carbons and hexadecyl
Pyridine reacts, and increases pore radius；Secondly, using carbon dioxide and the gaseous mixture of vapor in activated carbon activation process of the present invention
Body progress is physically activated, and the aperture of activated carbon has been widened under the synergistic effect of the two, the distribution of micropore and mesoporous is more closed
Reason, when making electrode material of the absorbent charcoal material as ultracapacitor, the electrochemistry of further raising ultracapacitor
Energy.
Embodiment
In order to describe the technical content, the structural feature, the achieved object and the effect of this invention in detail, below in conjunction with embodiment
It is explained in detail.
The design of most critical of the present invention is：Large aperture activated carbon of the present invention and preparation method thereof, first, the present invention use
Physics (ultrasonic wave) and chemistry (hydroxide corrosion) while act on carry out reaming, and in activation process using carbon dioxide and
The mixed gas progress of vapor is physically activated, and the aperture of activated carbon has been widened under the synergistic effect of the two.
The present invention provides a kind of preparation method of large aperture activated carbon, includes the following steps：
Step 1, crush activated carbon raw material, by the raw material soaking in ethanol solution, is additionally added in the ethanol solution
Hydroxide is expanding agent, and after supersonic oscillations, water washing dries to obtain Pre-Treatment of Activated charcoal；
Step 2, the Pre-Treatment of Activated charcoal add surfactant and 7-9h are impregnated at a temperature of 80-100 DEG C, are spaced 2-3h
Stirring, is uniformly mixed it；
Step 3, under nitrogen protection heat 2-4 it is small when, heating-up temperature be 300-500 degree, obtains Pre-Treatment of Activated charcoal, after general
Nitrogen switches to the mixed gas of vapor and carbon dioxide, when 700-800 degree soak times 1-3 is small, obtains large aperture work
Property charcoal.
The preparation method of above-mentioned large aperture activated carbon is made at the same time using physics (ultrasonic wave) and chemistry (hydroxide corrosion)
With reaming is carried out, the molecule of liquid is subject to transmitting for the energy of ultrasonic wave, interaction of molecules and produce substantial amounts of bubble, bubble
Rupture makes activated carbon capillary crush to form mesoporous.And hydroxide is dissolved in solution and as solution is diffused into activated carbon table
Corrosiveness is just played in face, this requires that the micropore of activated carbon allows for being soaked by liquid, and immersion is more abundant, and effect is better.
Activated Carbon Pretreatment is placed in cetylpyridinium chloride solution by the present invention, Surface Groups of Active Carbons and hexadecyl
Pyridine reacts, and increases pore radius.Secondly, physics work is carried out using the mixed gas of carbon dioxide and vapor in activation process
Change, the aperture of activated carbon has been widened under the synergistic effect of the two, has made the distribution of micropore and mesoporous more reasonable, makes the activated carbon
During electrode material of the material as ultracapacitor, the further chemical property for improving ultracapacitor.
Preferably, in the preparation method of above-mentioned large aperture activated carbon, the activated carbon raw material is wood activated charcoal or coconut palm
Shell activated carbon.
Preferably, in the preparation method of above-mentioned large aperture activated carbon, the hydroxide is the hydroxide of 1-2mol/L
Sodium or potassium hydroxide.
Preferably, in the preparation method of above-mentioned large aperture activated carbon, the frequency of the ultrasonic wave is 60-70Hz, vibration
When time is 1-2 small.
Preferably, in the preparation method of above-mentioned large aperture activated carbon, the surfactant is hexadecyl pyrrole
Pyridine.
Preferably, in the preparation method of above-mentioned large aperture activated carbon, the molar concentration of the surfactant is 10-
15mmol/L。
Preferably, in the preparation method of above-mentioned large aperture activated carbon, the Pre-Treatment of Activated charcoal and surfactant
Weight ratio is 1:1-2.
The present invention also provides large aperture activated carbon prepared by the preparation method of above-mentioned large aperture activated carbon.
Embodiment 1
A kind of preparation method of large aperture activated carbon, includes the following steps：
Step 1,100 mesh cocoanut active charcoals of selection are soaked in ethanol solution, and 1.5mol/ is further included in the ethanol solution
The potassium hydroxide of L, after supersonic oscillations, the frequency of the ultrasonic wave is 65Hz, when duration of oscillation is 1-2 small.Water washing
Dry to obtain Pre-Treatment of Activated charcoal；
Step 2, the Pre-Treatment of Activated charcoal add surfactant and 8h are impregnated at a temperature of 90 DEG C, and interval 2h stirrings, make
It is uniformly mixed；The surfactant is cetylpyridinium chloride.The molar concentration of the surfactant is 13mmol/
L.The weight ratio of the Pre-Treatment of Activated charcoal and surfactant is 1:1.
Step 3, under nitrogen protection heating 3 it is small when, heating-up temperature be 350 degree, obtain Pre-Treatment of Activated charcoal, after nitrogen is cut
Change the mixed gas of vapor and carbon dioxide into, when 750 degree of soak times 2 are small, obtain large aperture activated carbon.
Gained large aperture activated carbon specific surface area is 2730m2/ g, specific pore volume product 2.17ml/g, average pore size 18.25nm.
Embodiment 2
A kind of preparation method of large aperture activated carbon, includes the following steps：
Step 1,80 mesh cocoanut active charcoals of selection are soaked in ethanol solution, further include 1mol/L's in the ethanol solution
Potassium hydroxide, after supersonic oscillations, the frequency of the ultrasonic wave is 60Hz, when duration of oscillation is 1 small.Water washing is dried
Pre-Treatment of Activated charcoal；
Step 2, the Pre-Treatment of Activated charcoal add surfactant and 7h are impregnated at a temperature of 80 DEG C, and interval 2h stirrings, make
It is uniformly mixed；The surfactant is cetylpyridinium chloride.The molar concentration of the surfactant is 10mmol/
L.The weight ratio of the Pre-Treatment of Activated charcoal and surfactant is 1:1.
Step 3, under nitrogen protection heating 2 it is small when, heating-up temperature be 300 degree, obtain Pre-Treatment of Activated charcoal, after nitrogen is cut
Change the mixed gas of vapor and carbon dioxide into, when 700 degree of soak times 1 are small, obtain large aperture activated carbon.
Gained large aperture activated carbon specific surface area is 2830m2/ g, specific pore volume product 2.07ml/g, average pore size 17.26nm.
Embodiment 3
A kind of preparation method of large aperture activated carbon, includes the following steps：
Step 1,90 mesh cocoanut active charcoals of selection are soaked in ethanol solution, further include 2mol/L's in the ethanol solution
Potassium hydroxide, after supersonic oscillations, the frequency of the ultrasonic wave is 70Hz, when duration of oscillation is 1-2 small.Water washing is dried
Obtain Pre-Treatment of Activated charcoal；
Step 2, the Pre-Treatment of Activated charcoal add surfactant and 9h are impregnated at a temperature of 100 DEG C, and interval 3h stirrings, make
It is uniformly mixed；The surfactant is cetylpyridinium chloride.The molar concentration of the surfactant is 15mmol/
L.The weight ratio of the Pre-Treatment of Activated charcoal and surfactant is 1:2.
Step 3, under nitrogen protection heating 4 it is small when, heating-up temperature be 500 degree, obtain Pre-Treatment of Activated charcoal, after nitrogen is cut
Change the mixed gas of vapor and carbon dioxide into, when 800 degree of soak times 3 are small, obtain large aperture activated carbon.
Gained large aperture activated carbon specific surface area is 2730m2/ g, specific pore volume product 2.35ml/g, average pore size 18.55nm.
The foregoing is merely the embodiment of the present invention, is not intended to limit the scope of the invention, every to utilize this hair
The equivalent structure or equivalent flow shift that bright specification is made, is directly or indirectly used in other related technical areas,
Similarly it is included within the scope of the present invention.
Claims (8)
1. a kind of preparation method of large aperture activated carbon, it is characterised in that include the following steps：
Step 1, crush activated carbon raw material, and by the raw material soaking in ethanol solution, hydrogen-oxygen is additionally added in the ethanol solution
Compound is expanding agent, and after supersonic oscillations, water washing dries to obtain Pre-Treatment of Activated charcoal；
Step 2, the Pre-Treatment of Activated charcoal add surfactant and 7-9h are impregnated at a temperature of 80-100 DEG C, and interval 2-3h is stirred
Mix, be uniformly mixed it；
Step 3, heat under nitrogen protection 2-4 it is small when, heating-up temperature is 300-500 degree, obtains Pre-Treatment of Activated charcoal, after by nitrogen
The mixed gas of vapor and carbon dioxide is switched to, when 700-800 degree soak times 1-3 is small, obtains large aperture activated carbon.
2. the preparation method of large aperture activated carbon according to claim 1, it is characterised in that the activated carbon raw material is wood
Activated carbon or cocoanut active charcoal.
3. the preparation method of large aperture activated carbon according to claim 1, it is characterised in that the hydroxide is 1-
The sodium hydroxide or potassium hydroxide of 2mol/L.
4. the preparation method of large aperture activated carbon according to claim 1, it is characterised in that the frequency of the ultrasonic wave is
60-70Hz, when duration of oscillation is 1-2 small.
5. the preparation method of large aperture activated carbon according to claim 1, it is characterised in that the surfactant is chlorine
Change cetyl pyridinium.
6. the preparation method of large aperture activated carbon according to claim 5, it is characterised in that the surfactant rubs
Your concentration is 10-15mmol/L.
7. the preparation method of large aperture activated carbon according to claim 6, it is characterised in that the Pre-Treatment of Activated charcoal with
The weight ratio of surfactant is 1:1-2.
8. large aperture activated carbon prepared by a kind of preparation method of claim 1-7 any one of them large aperture activated carbon.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108946725A (en) * | 2018-07-19 | 2018-12-07 | 深圳市环球绿地新材料有限公司 | Spherical activated charcoal, the preparation method and use of loading cation surfactant |
| WO2020155856A1 (en) | 2019-01-28 | 2020-08-06 | 贵州梅岭电源有限公司 | Method for preparing stalactite-like macroporous activated carbon |
| CN112575575A (en) * | 2020-07-21 | 2021-03-30 | 苏州远浩新纺织科技有限公司 | Hole expanding method for activated carbon fiber |
| CN112588263A (en) * | 2020-11-30 | 2021-04-02 | 德清县联新环保科技有限公司 | Regenerated active carbon and preparation method thereof |
| CN112730726A (en) * | 2020-12-29 | 2021-04-30 | 中冶建筑研究总院有限公司 | Method for measuring content of metal loaded in catalyst |
| CN115888786A (en) * | 2022-10-26 | 2023-04-04 | 鄂尔多斯市瀚博科技有限公司 | Si-modified acetylene hydrochlorination metal-free catalyst, preparation method and application |
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| CN102442665A (en) * | 2011-09-28 | 2012-05-09 | 福州大学 | Thermally treated active carbon and preparation method thereof |
| CN103721675A (en) * | 2013-12-20 | 2014-04-16 | 同济大学 | Modifying method for cationic surface active agent modified activated carbon and application of cationic surface active agent modified activated carbon |
| CN104891492A (en) * | 2015-06-15 | 2015-09-09 | 威海文隆电池有限公司 | Preparation method for activated carbon with medium pore radii |
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2017
- 2017-11-28 CN CN201711215807.7A patent/CN107973296A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102442665A (en) * | 2011-09-28 | 2012-05-09 | 福州大学 | Thermally treated active carbon and preparation method thereof |
| CN103721675A (en) * | 2013-12-20 | 2014-04-16 | 同济大学 | Modifying method for cationic surface active agent modified activated carbon and application of cationic surface active agent modified activated carbon |
| CN104891492A (en) * | 2015-06-15 | 2015-09-09 | 威海文隆电池有限公司 | Preparation method for activated carbon with medium pore radii |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108946725A (en) * | 2018-07-19 | 2018-12-07 | 深圳市环球绿地新材料有限公司 | Spherical activated charcoal, the preparation method and use of loading cation surfactant |
| WO2020155856A1 (en) | 2019-01-28 | 2020-08-06 | 贵州梅岭电源有限公司 | Method for preparing stalactite-like macroporous activated carbon |
| CN112575575A (en) * | 2020-07-21 | 2021-03-30 | 苏州远浩新纺织科技有限公司 | Hole expanding method for activated carbon fiber |
| WO2022016663A1 (en) * | 2020-07-21 | 2022-01-27 | 苏州远浩新纺织科技有限公司 | Reaming method for activated carbon fiber |
| CN112588263A (en) * | 2020-11-30 | 2021-04-02 | 德清县联新环保科技有限公司 | Regenerated active carbon and preparation method thereof |
| CN112730726A (en) * | 2020-12-29 | 2021-04-30 | 中冶建筑研究总院有限公司 | Method for measuring content of metal loaded in catalyst |
| CN112730726B (en) * | 2020-12-29 | 2023-10-24 | 中冶建筑研究总院有限公司 | Method for measuring content of metal loaded in catalyst |
| CN115888786A (en) * | 2022-10-26 | 2023-04-04 | 鄂尔多斯市瀚博科技有限公司 | Si-modified acetylene hydrochlorination metal-free catalyst, preparation method and application |
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