CN109502585A - A kind of preparation method for the high-specific surface area activated carbon from activated sludge that magnesium is nitrogen co-doped - Google Patents
A kind of preparation method for the high-specific surface area activated carbon from activated sludge that magnesium is nitrogen co-doped Download PDFInfo
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- CN109502585A CN109502585A CN201811614360.5A CN201811614360A CN109502585A CN 109502585 A CN109502585 A CN 109502585A CN 201811614360 A CN201811614360 A CN 201811614360A CN 109502585 A CN109502585 A CN 109502585A
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- C01—INORGANIC CHEMISTRY
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- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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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
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- C01B32/342—Preparation characterised by non-gaseous activating agents
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Abstract
The invention discloses a kind of preparation method and applications of high-specific surface area biomass active Carbon Materials that magnesium is nitrogen co-doped.The active carbon has the three-dimensional composite pore structural of unique foramen magnum-mesoporous-micropore, and feature is that magnesium is nitrogen co-doped.This method after over cleaning, drying, shearing pretreatment, the mixed solution time of infusion of raw material and zinc chloride and magnesium chloride is fitted into tube furnace after drying, in a nitrogen atmosphere carbonization-activation and cooling using the big hemp core of biomass waste material as raw material.After gains are carried out pickling and washing, dry in the ethanol solution of aminopyridine after time of infusion to get the active carbon nitrogen co-doped to the magnesium.The specific surface area of the active carbon is high, shows excellent carbon dioxide gas absorption property.
Description
Technical field
The present invention relates to a kind of method for preparing active carbon as raw material using biomass waste material, especially one kind to be with biomass
The method that raw material prepares the nitrogen co-doped high-specific surface area activated carbon from activated sludge of magnesium.
Background technique
The large specific surface area of active carbon, strong adsorption, have been widely used for chemical industry, environmental protection, food processing, metallurgy,
The every field such as drug purification and military chemistry protection.Traditional active carbon is mainly using fat coal as raw material, higher cost.In order to
Reduce cost, at the same it is energy saving, preserve the ecological environment, exploitation has important show by the active carbon of raw material of renewable resource
Sincere justice.
Hemp has the characteristics that low cost, high yield, low nutrient demand, high land utilization ratio, is a kind of environmental-friendly
Crop.Hemp is the main source of the industry such as papermaking, weaving and rope.In the industrial production, hemp phloem is for producing fiber.
After big waste of flax sloughs bast, remaining wooden core is big hemp core.Bast fiber usually only accounts for 25% mass parts or so of big waste of flax,
A large amount of big hemp core becomes biological waste as by-product.Big hemp core by 40-48% cellulose, 18-24% hemicellulose and
21-24% lignin composition is the production extraordinary carbon source of active carbon.
It is of great significance in consideration of it, providing a kind of method for preparing active carbon with high specific surface area as raw material using big hemp core.
Summary of the invention
The object of the present invention is to provide a kind of preparation sides of high-specific surface area activated carbon from activated sludge that magnesium is nitrogen co-doped
Method, the present invention prepare active carbon using the big hemp core of biomass waste material as raw material, and raw material is easy to get at low cost.And the active carbon being prepared
Middle magnesium is nitrogen co-doped, and specific surface area is high, and performance is good.
To achieve the goals above, the technical solution adopted by the present invention are as follows: a kind of high-specific surface area that magnesium is nitrogen co-doped is raw
The preparation method of species activity charcoal, comprising the following steps:
(1) by after big hemp core cleaning, drying, it is cut into segment；
(2) big hemp core segment is placed in the mixed aqueous solution of zinc chloride and magnesium chloride after being sufficiently impregnated and is filtered, then existed
Dry 12-26h at 78 DEG C -82 DEG C；
(3) by the big hemp core segment after drying under inert gas protection high temperature sintering and keep the temperature a period of time, then exist
Natural cooling under inert gas shielding, obtains carbide；
(4) it by carbide with after vacuum decompression pickling 10-14h, then is washed with distilled water, reaches PH neutrality；
(5) after carbide obtained by step (4) being sufficiently impregnated in the ethanol solution of aminopyridine compounds, 78 DEG C-
Dry 12-26h, obtains the nitrogen co-doped high-specific surface area activated carbon from activated sludge of the magnesium at 82 DEG C.
The preparation method of the nitrogen co-doped high-specific surface area activated carbon from activated sludge of magnesium above-mentioned, in the step (1), cleaning
Drying temperature afterwards is 98 DEG C -102 DEG C, and big hemp core is cut into the segment that length is 1-5cm.
The preparation method of the nitrogen co-doped high-specific surface area activated carbon from activated sludge of magnesium above-mentioned, in step (2), the mixing
In aqueous solution, the concentration of zinc chloride and magnesium chloride mixture solution is 20-60%.
The preparation method of the nitrogen co-doped high-specific surface area activated carbon from activated sludge of magnesium above-mentioned, in step (2), the mixing
The mass ratio of zinc chloride and magnesium chloride is 1:1-4:1 in aqueous solution, and zinc chloride and the big hemp core mass ratio impregnated are 2:1-4:
1, the dip time of big hemp core is 18-48h.
The preparation method of the nitrogen co-doped high-specific surface area activated carbon from activated sludge of magnesium above-mentioned, in step (3), inert gas
For nitrogen or argon gas.
The preparation method of the nitrogen co-doped high-specific surface area activated carbon from activated sludge of magnesium above-mentioned, in step (3), the height
Temperature is sintered and keeps the temperature；It is warming up to 400-900 DEG C of progress high temperature sintering with the speed of 5-10 DEG C/min, keeps the temperature 2-
5h。
The preparation method of the nitrogen co-doped high-specific surface area activated carbon from activated sludge of magnesium above-mentioned, in rapid (4), the pickling
Acid used is one or more of dilute hydrochloric acid, dilute sulfuric acid or dust technology.
The preparation method of the nitrogen co-doped high-specific surface area activated carbon from activated sludge of magnesium above-mentioned, in step (5), the ammonia
Yl pyridines compound is 2-aminopyridine, 2,3- diamino-pyridines, one or more of 2,6-diaminopyridine.
The preparation method of the nitrogen co-doped high-specific surface area activated carbon from activated sludge of magnesium above-mentioned, in step (5), the ammonia
In the ethanol solution of yl pyridines compound, the concentration of aminopyridine compounds is 0.2-0.5g/ml.
The preparation method of the nitrogen co-doped high-specific surface area activated carbon from activated sludge of magnesium above-mentioned, in step (5), when dipping,
Dip time is 4h-12h.
Compared with prior art, the invention has the following advantages:
1, the present invention produces active carbon by raw material of big hemp core, is the method for a kind of low cost and easy processing, realizes simultaneously
The comprehensive utilization of waste.Big hemp core has unique three-dimensional communication pore structure, and active carbon made from it has unique
The three-dimensional composite pore structural of foramen magnum-mesoporous-micropore is both efficient absorption body and good hetero atom carrier.
2, the active carbon nitrogen co-doped as the magnesium of raw material using big hemp core that the present invention announces, in the carbonization-activation mistake of big hemp core
Magnesia and aminopyridine are introduced in journey, the codope of magnesium and nitrogen on the activated carbon plays synergistic effect, improves active carbon to two
The adsorption capacity of carbonoxide.Also have having been widely used in basins such as capacitor, electrode materials, is not only limited to of the present invention
Adsorbing domain.Then nitrogen is introduced in molding activated carbon surface.The large specific surface area of gained active carbon, magnesium and nitrogen are total to
Synergistic effect has been adulterated, has improved active carbon to the adsorption capacity of carbon dioxide.
3, the present invention is using big hemp core as raw material, while realizing the recycling of biomass waste material, the work being prepared
Property charcoal have unique foramen magnum-mesoporous-micropore three-dimensional composite holes microstructure, large specific surface area, favorable repeatability.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of hemp core raw material used in the present invention, the cross section (a) and the longitudinal section (b) of big hemp core
Scanning electron microscope (SEM) photograph.
Specific embodiment
The present invention is described in further details combined with specific embodiments below, but the present invention is not limited thereto.
Embodiment 1:
A kind of preparation method for the high-specific surface area activated carbon from activated sludge that magnesium is nitrogen co-doped: specific as follows: big hemp core (scanning
Electron microscope is shown in Fig. 1) wash with distilled water after, dried at 100 DEG C, and be cut into the segment of about 3cm；By big hemp core segment in chlorination
It is impregnated in the water mixed solution of zinc and magnesium chloride, the concentration of mixed aqueous solution is 50%, zinc chloride and chlorination in mixed aqueous solution
The mass ratio of magnesium is 4:1, and zinc chloride and the big hemp core mass ratio impregnated are 4:1.After decompression impregnates for 24 hours in a vacuum drying oven
Then filtering is dried for 24 hours at 80 DEG C.Big hemp core after drying is placed in tube furnace, in a nitrogen atmosphere, with 5 DEG C/min
Speed be warming up to 600 DEG C, and keep the temperature 2h at 600 DEG C, be then cooled to room temperature in a nitrogen atmosphere.The carbide that will be obtained
It is impregnated with dilute hydrochloric acid solution (concentration 1mol/L), PH is washed with distilled water to after vacuum decompression pickling 12h again as neutrality.After filtering
By gained carbide in the ethanol solution of 2,6-diaminopyridine after (concentration 0.3g/ml) decompression dipping 6h, at 80 DEG C
Drying is for 24 hours to get the active carbon nitrogen co-doped to magnesium.The active carbon specific surface area is up to 3128m2/ g, to carbon dioxide (25
DEG C, 1bar) adsorbance be up to 5.87mmol/g.
Embodiment 2:
A kind of preparation method for the high-specific surface area activated carbon from activated sludge that magnesium is nitrogen co-doped: specific as follows: big hemp core steams
After distilled water cleaning, dried at 100 DEG C, and be cut into the segment of 3cm.Big hemp core segment is molten in the mixing of zinc chloride and magnesium chloride
It is impregnated in liquid.The concentration of mixed solution is 50%, and the mass ratio of zinc chloride and magnesium chloride is 4:1 in mixed solution, zinc chloride and
The big hemp core mass ratio impregnated is 2:1.Decompression dipping filters afterwards for 24 hours in a vacuum drying oven, then dry at 80 DEG C
24h.Big hemp core after drying is placed in tube furnace, in a nitrogen atmosphere, is warming up to 800 DEG C with the speed of 5 DEG C/min, and
2h is kept the temperature at 800 DEG C, is then cooled to room temperature in a nitrogen atmosphere.By obtained carbide dilute hydrochloric acid solution (concentration 1mol/
L it) impregnates, PH is washed with distilled water to after vacuum decompression pickling 12h again as neutrality.By gained carbide in 2- amino pyrrole after filtering
It is dry for 24 hours to get nitrogen co-doped to magnesium at 80 DEG C in the ethanol solution of pyridine after (concentration 0.5g/ml) decompression dipping 6h
Active carbon.The active carbon specific surface area is up to 2930m2/ g is up to the adsorbance of carbon dioxide (25 DEG C, 1bar)
5.49mmol/g。
Claims (10)
1. a kind of preparation method for the high-specific surface area activated carbon from activated sludge that magnesium is nitrogen co-doped, it is characterised in that: including following step
It is rapid:
(1) by after big hemp core cleaning, drying, it is cut into segment；
(2) big hemp core segment is placed in the mixed aqueous solution of zinc chloride and magnesium chloride after being sufficiently impregnated and is filtered, then 78 DEG C-
Dry 12-26h at 82 DEG C；
(3) by the big hemp core segment after drying under inert gas protection high temperature sintering and keep the temperature a period of time, then in inertia
Natural cooling under gas shield, obtains carbide；
(4) it by carbide with after vacuum decompression pickling 10-14h, then is washed with distilled water, reaches PH neutrality；
(5) after being sufficiently impregnated carbide obtained by step (4) in the ethanol solution of aminopyridine compounds, at 78 DEG C -82 DEG C
Lower dry 12-26h obtains the nitrogen co-doped high-specific surface area activated carbon from activated sludge of the magnesium.
2. the preparation method of the nitrogen co-doped high-specific surface area activated carbon from activated sludge of magnesium as described in claim 1, feature exist
In: in the step (1), the drying temperature after cleaning is 98 DEG C -102 DEG C, and big hemp core is cut into the segment that length is 1-5cm.
3. the preparation method of the nitrogen co-doped high-specific surface area activated carbon from activated sludge of magnesium as described in claim 1, feature exist
In: in step (2), in the mixed aqueous solution, the concentration of zinc chloride and magnesium chloride mixture solution is 20-60%.
4. the preparation method of the nitrogen co-doped high-specific surface area activated carbon from activated sludge of magnesium as described in claim 1, feature exist
In: in step (2), the mass ratio of zinc chloride and magnesium chloride is 1:1-4:1 in the mixed aqueous solution, zinc chloride and is impregnated
Big hemp core mass ratio is 2:1-4:1, and the dip time of big hemp core is 18-48h.
5. the preparation method of the nitrogen co-doped high-specific surface area activated carbon from activated sludge of magnesium as described in claim 1, feature exist
In: in step (3), inert gas is nitrogen or argon gas.
6. the preparation method of the nitrogen co-doped high-specific surface area activated carbon from activated sludge of magnesium as described in claim 1: its feature exists
In: in step (3), the high temperature sintering simultaneously keeps the temperature and is for a period of time；400-900 DEG C is warming up to the speed of 5-10 DEG C/min
High temperature sintering is carried out, 2-5h is kept the temperature.
7. the preparation method of the nitrogen co-doped high-specific surface area activated carbon from activated sludge of magnesium as described in claim 1, feature exist
In: in institute rapid (4), acid used in the pickling is one or more of dilute hydrochloric acid, dilute sulfuric acid or dust technology.
8. the preparation method of the nitrogen co-doped high-specific surface area activated carbon from activated sludge of magnesium as described in claim 1, feature exist
In: in step (5), the aminopyridine compounds are 2-aminopyridine, 2,3- diamino-pyridines, in 2,6-diaminopyridine
More than one.
9. the preparation method of the nitrogen co-doped high-specific surface area activated carbon from activated sludge of magnesium as described in claim 1, feature exist
In: in step (5), in the ethanol solution of the aminopyridine compounds, the concentration of aminopyridine compounds is 0.2-0.5g/
ml。
10. the preparation method of the nitrogen co-doped high-specific surface area activated carbon from activated sludge of magnesium as described in claim 1, feature exist
In: in step (5), when dipping, dip time 4h-12h.
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| CN201811614360.5A CN109502585B (en) | 2018-12-27 | 2018-12-27 | Preparation method of magnesium-nitrogen-codoped high-specific-surface-area biomass activated carbon |
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| CN201811614360.5A CN109502585B (en) | 2018-12-27 | 2018-12-27 | Preparation method of magnesium-nitrogen-codoped high-specific-surface-area biomass activated carbon |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114836769A (en) * | 2022-06-10 | 2022-08-02 | 浙江工业大学 | 2, 6-diaminopyridine/silver porous photoelectrode material and preparation method and application thereof |
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