CN107555433A - Anthracite nitrating activated carbon and preparation method thereof - Google Patents
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Abstract
The present invention provides a kind of anthracite nitrating activated carbon and preparation method thereof, comprises the following steps：The anchracite duff for removing impurity is broken into powder first, powder is dried；Dried anthracite powder is transferred in quartz ampoule after being well mixed with activator, is passed through nitrogen or inert gas purge quartz ampoule and sample, nitrogen source is then passed through in quartz ampoule, then carries out carbonization treatment and activation process obtains nitrating activated carbon；Above-mentioned nitrating activated carbon is washed with watery hydrochloric acid, is dried to obtain anthracite nitrating activated carbon product；The present invention obtains high-quality nitrating activated carbon with traditional coal by simple industrialization processing, the nitrating activated carbon of preparation can be applied in the energy storage field such as ultracapacitor field, and the process that the present invention uses is simple, equipment requirement is low, ensure that material can large-scale industrial production, and material quality is reliable and stable, and uniformity is good, preparation method is simple, and cost is low.
Description
Technical field
The present invention relates to active carbon from coal technical field, and in particular to a kind of anthracite nitrating activated carbon and its preparation side
Method.
Background technology
Coal resources are mainly still used for traditional fuel at present, and traditional fuel resource is also to cause adding for Global Greenhouse Effect
Acute main cause, the development and exploitation of new energy, it is a kind of new environment-friendly materials by coal exploitation as global environment is renovated
It is an imperative trend.With the fast development of new energy and energy storage industry, active carbon from coal is one more good
Selection.The exploitation of current active carbon from coal has been obtained for the extensive concern of researcher, and raw coal screen clearly
Washing the active carbon from coal that rear crystal orientation heat treatment obtains has the specific surface area of superelevation, to organic in some gases, liquid
Thing or inorganic matter have superpower adsorption capacity, while have good physical and chemical stability, and good mechanical strength is resistance to
It is sour, alkaline-resisting and heat-resisting, can be as the adsorbent of many materials insoluble in organic solvent and water, and may be reused.
Active carbon from coal also has relative to other carbon materials, such as timber, shell, coconut husk, walnut shell, apricot shell, jujube shell
Obvious advantage, the anthracite that particularly present invention selects have very high carbon content, produced in the preparation process of activated carbon
Product yield is very high, is advantageous to industrialized production.The processing mode of activated carbon generally uses traditional heating mode at present, by raw material with
Activator is heated after being mixed according to certain ratio, and need long-time keeping temperature, this activated carbon for preparing
The mode reaction time is longer, and it is big to consume energy, and is unfavorable for industrialization large-scale production.
Microwave technology has the incomparable advantage of traditional heating, traditional heating mode as a kind of new heating technique
It is that material is progressively heated up by external heat source, in order to avoid material structure destroys in heating process, firing rate is often
Can not be too fast, selective heating can not be carried out to mixture each component in unified reaction unit, but microwave heats can
Avoid these problems.It is that volume heats caused by dielectric loss itself in material electromagnetic field because microwave heats, therefore can be real
Existing molecular level stirring, heating is more uniform, and because different materials molecular structure is different, microwave heating also have selection plus
The characteristics of hot.In heating process, the power of microwave can as needed quick regulation, be easy to that control, firing rate is fast, thermal effect
Rate is high, is to industrialize the optimal selection produced automatically.
The purposes of activated carbon mainly forms decision by its specific surface area and composition, at present active carbon from coal single varieties,
Purposes needs further to be developed.
The content of the invention
Influenceed for traditional coal carbonization stone fuel to caused by global warming and the problems such as air pollution, the present invention
Purpose be to develop a kind of absorbent charcoal material prepared as raw material using anthracite, by traditional coal industry and new energy industry
Organically combine, using anthracite and activator and nitrogen source as raw material, control preparation condition prepare a kind of high-quality without
Bituminous coal nitrating activated carbon.
For achieving the above object, technical solution of the present invention is as follows：
A kind of preparation method of anthracite nitrating activated carbon, comprises the following steps：
(1) anchracite duff for removing impurity is broken into powder first, then dried powder；
(2) dried anthracite powder is transferred in quartz ampoule after being well mixed with activator, anthracite powder and work
Agent mass ratio is 1:(1-4)；
(3) nitrogen or inert gas purge quartz ampoule and sample are passed through, nitrogen source is then passed through in quartz ampoule, is then carried out
Carbonization treatment and activation process obtain nitrating activated carbon；
(4) above-mentioned nitrating activated carbon is fully washed with watery hydrochloric acid, then repeatedly washed with water, be finally dried to obtain anthracite
Nitrating activated carbon product.
It is preferred that its particle diameter is less than 800 microns after anthracite powder crushes in step (1), drying temperature 80-
120 DEG C, drying time is 8-15 hours.
It is preferred that the activator of step (2) is included in potassium hydroxide, zinc chloride, iron chloride, sodium hydroxide at least
It is a kind of.
It is preferred that step (2) anthracite powder adds water during being mixed with activator obtains slurry, wherein
The mass ratio 1 of activator and water:1, obtained slurry, which evaporates 3-6 hours in 60 DEG C, goes out most of moisture, then by slurry in
80 DEG C of dryings 24 hours, are then transferred into quartz ampoule.
It is preferred that the nitrogen source that step (3) uses is ammonia, magnesium nitride is at least one.
It is preferred that step (3) carries out activation process with microwave irradiation, microwave irradiation power is 400-1200W, micro-
The time that amplitude is shone is 6-20 minutes.
It is preferred that step (3) activation process is carried out with carbonization treatment simultaneously, carburizing temperature is 500-1200 DEG C.
It is preferred that step (4) nitrating activated carbon concentration is the salt acid elution that 0.8-1.6mol/ rises, washing
Time is 10-20 hours, and wash temperature is 50-70 DEG C, then is repeatedly washed with water, and the drying temperature after washing is 70-120 DEG C,
Drying time is more than 10 hours.
It is preferred that collecting clean anthracite raw material before step (1), first anthracite is crushed to
Ball milling is being carried out after 0.2cm particle diameters, is making its particle diameter smaller, is easy to be sufficiently mixed with activator.
The anthracite nitrating activated carbon yield that the inventive method obtains is 47.1%~75.3%.
For achieving the above object, the present invention also provides the anthracite nitrating activity that a kind of above-mentioned preparation method obtains
Charcoal.
The anthracite nitrating activated carbon of gained is inhaled to the adsorbance of methylene blue in 340.9mg/g~1233.5mg/g, iodine
Attached amount is 34.5mg/g~146.8mg/g；Anthracite nitrating activated carbon BET specific surface area is 779.85m2/ g~1750m2/ g, always
Pore volume is 0.401cm3/ g~0.589cm3/ g, average pore size 1-9nm.
The present invention carries out N doping while using novel microwave heating synthesis active carbon from coal using nitrogen, obtains
N doping active carbon from coal, it is set to be expected to be used for the energy-storage property that capacitor is improved in ultracapacitor field.The present invention is through tradition
Coal obtains high-quality nitrating activated carbon by simple industrialization processing, by activated carbon application ultracapacitor field, through tradition
The energy organically combines with new energy, realizes the industrial chain of Green Sustainable, and the experiment that the present invention uses
Journey is simple, and equipment requirement is low, ensure that material being capable of large-scale industrial production.
A kind of nitrating anthracite method for preparation of active carbon of the present invention, compared with existing coal based activated Carbon Materials, what it was protruded
Feature and excellent effect are：
1. the present invention obtains high-quality nitrating activated carbon with traditional coal by simple industrialization processing, the nitrating of preparation is lived
Property charcoal can apply in the energy storage field such as ultracapacitor field, organically combined through traditional energy with new energy, realize
The industrial chain of Green Sustainable, and the experimentation that the present invention uses is simple, equipment requirement is low, ensure that material is energy
Enough large-scale industrial productions.
2. the preparing raw material source of the present invention is conventional fossil fuel, but the direct burning of fossil fuel can cause a system
Row environmental issue, but the generation of this problem can be avoided by the present invention, and also material quality is reliable and stable, uniformity
Good, preparation method is simple, and cost is low, and technology of preparing is simple, and exploitativeness is strong, and industrialization difficulty is small, it is possible to achieve extensive raw
Production.
Brief description of the drawings
Fig. 1 is the SEM figures of nitrating anthracite activated carbon prepared by the present invention.
Embodiment
Illustrate embodiments of the present invention below by way of specific instantiation, those skilled in the art can be by this specification
Disclosed content understands other advantages and effect of the present invention easily.The present invention can also pass through specific realities different in addition
The mode of applying is embodied or practiced, the various details in this specification can also be based on different viewpoints with application, without departing from
Various modifications or alterations are carried out under the spirit of the present invention.
Embodiment 1
A kind of preparation method of anthracite nitrating activated carbon, comprises the following steps：
(1) clean anthracite raw material is collected, impurity is removed, anchracite duff is broken into powder, its particle diameter is less than after crushing
800 microns, it is easy to be sufficiently mixed with activator, then dries powder；Drying temperature is 80 DEG C, and drying time is 8 small
When.
(2) dried anthracite powder mixes with activator, and activator is potassium hydroxide, anthracite powder and activator
Mass ratio is 1:1；Water is added during mixing and obtains the mass ratio 1 of slurry, wherein activator and water:1, obtained slurry
3 hours most of moisture of going out are evaporated in 60 DEG C, then slurry is dried 24 hours in 80 DEG C, quartz ampoule is transferred to after well mixed
In.
(3) nitrogen cleaning quartz ampoule and sample are passed through, nitrogen source ammonia is then passed through in quartz ampoule, is then carried out at carbonization
Reason and activation process obtain nitrating activated carbon；Activation process is carried out with microwave irradiation, and microwave irradiation power is 400W, microwave irradiation
Time be 6 minutes, activation process is carried out simultaneously with carbonization treatment, carburizing temperature be 500 DEG C.
(4) it is that the salt pickling that 0.8mol/ rises fully is washed with concentration by above-mentioned nitrating activated carbon, wash time is 10 small
When, wash temperature is 50 DEG C, then is repeatedly washed with water, is then dried, and drying temperature is 70 DEG C, and drying time is more than 10 hours,
Obtain anthracite nitrating activated carbon product.
The anthracite nitrating activated carbon yield that the inventive method obtains is 47.1%~75.3%.The anthracite nitrating of gained
For activated carbon to the adsorbance of methylene blue in 340.9mg/g~1233.5mg/g, iodine absorption number is 34.5mg/g~146.8mg/
g；Anthracite nitrating activated carbon BET specific surface area is 779.85m2/ g~1750m2/ g, total pore volume 0.401cm3/ g~
0.589cm3/ g, average pore size 1-9nm.
Embodiment 2
A kind of preparation method of anthracite nitrating activated carbon, comprises the following steps：
(1) clean anthracite raw material is collected, impurity is removed, anthracite is crushed to after 0.2cm particle diameters and carries out ball milling again,
Anchracite duff is broken into powder to be easy to be sufficiently mixed with activator, then dried powder；Drying temperature is 120 DEG C, is done
The dry time is 15 hours.
(2) dried anthracite powder mixes with activator, and activator is zinc chloride, anthracite powder and activator matter
Amount is than being 1:4；Water is added during mixing and obtains the mass ratio 1 of slurry, wherein activator and water:1, obtained slurry in
60 DEG C of evaporations, 6 hours most of moisture of going out, then slurry is dried 24 hours in 80 DEG C, it is transferred to quartz ampoule after well mixed
In.
(3) inert gas purge quartz ampoule and sample are passed through, nitrogen source magnesium nitride is then passed through in quartz ampoule.Then carry out
Carbonization treatment and activation process obtain nitrating activated carbon；Activation process is carried out with microwave irradiation, microwave irradiation power is 1200W,
The time of microwave irradiation is 20 minutes.Activation process is carried out simultaneously with carbonization treatment, and carburizing temperature is 1200 DEG C.
(4) it is that the hydrochloric acid that 1.6mol/ rises fully washs with concentration by above-mentioned nitrating activated carbon, wash time 20 hours, washes
Temperature is washed as 70 DEG C, then is repeatedly washed with water, is then dried, drying temperature is 120 DEG C, and drying time is more than 10 hours, obtains
Anthracite nitrating activated carbon product.
Obtained anthracite nitrating activated carbon yield is 47.1%~75.3%.The anthracite nitrating activated carbon of gained is to Asia
For the adsorbance of methyl blue in 340.9mg/g~1233.5mg/g, iodine absorption number is 34.5mg/g~146.8mg/g；Anthracite is mixed
Nitrogen activated carbon BET specific surface area is 779.85m2/ g~1750m2/ g, total pore volume 0.401cm3/ g~0.589cm3/ g, it is average
Aperture is 1-9nm.
Embodiment 3
A kind of preparation method of anthracite nitrating activated carbon, comprises the following steps：
(1) clean anthracite raw material is collected, impurity is removed, anchracite duff is broken into powder, its particle diameter is less than after crushing
800 microns, it is easy to be sufficiently mixed with activator, then dries powder；Drying temperature is 100 DEG C, drying time 10
Hour.
(2) dried anthracite powder mixes with activator, and activator is iron chloride, anthracite powder and activator matter
Amount is than being 1:2；Water is added during mixing and obtains the mass ratio 1 of slurry, wherein activator and water:1, obtained slurry in
60 DEG C of evaporations, 4 hours most of moisture of going out, then slurry is dried 24 hours in 80 DEG C, it is transferred to quartz ampoule after well mixed
In.
(3) nitrogen or inert gas purge quartz ampoule and sample are passed through, nitrogen source is then passed through in quartz ampoule, nitrogen source is ammonia
Gas and magnesium nitride.Then carry out carbonization treatment and activation process obtains nitrating activated carbon；Activation process is carried out with microwave irradiation, it is micro-
Ripple irradiation power is 800W, and the time of microwave irradiation is 10 minutes.Activation process is carried out simultaneously with carbonization treatment, and carburizing temperature is
800℃。
(4) above-mentioned nitrating activated carbon is fully washed with watery hydrochloric acid, step (4) nitrating activated carbon concentration is
The salt acid elution that 1.2mol/ rises, wash time are 14 hours, and wash temperature is 60 DEG C, then is repeatedly washed with water, finally dry
To anthracite nitrating activated carbon product.Drying temperature after washing is 90 DEG C, and drying time is more than 10 hours.
Obtained anthracite nitrating activated carbon yield is 47.1%~75.3%.The anthracite nitrating activated carbon of gained is to Asia
For the adsorbance of methyl blue in 340.9mg/g~1233.5mg/g, iodine absorption number is 34.5mg/g~146.8mg/g；Anthracite is mixed
Nitrogen activated carbon BET specific surface area is 779.85m2/ g~1750m2/ g, total pore volume 0.401cm3/ g~0.589cm3/ g, it is average
Aperture is 1-9nm.
Embodiment 4
A kind of preparation method of anthracite nitrating activated carbon, comprises the following steps：
(1) clean anthracite raw material is collected, impurity is removed, anthracite is crushed to after 0.2cm particle diameters and carries out ball milling again,
Anchracite duff is broken into powder, is easy to be sufficiently mixed with activator, then dries powder；Drying temperature is 110 DEG C, is done
The dry time is 12 hours.
(2) dried anthracite powder mixes with activator, and activator includes potassium hydroxide, zinc chloride, sodium hydroxide,
Anthracite powder is 1 with activator mass ratio:3；Water is added during mixing and obtains the quality of slurry, wherein activator and water
Ratio 1:1, obtained slurry evaporates 5 hours most of moisture of going out in 60 DEG C, then slurry is dried 24 hours in 80 DEG C, mixing
It is transferred to after uniformly in quartz ampoule.
(3) argon purge quartz ampoule and sample are passed through, nitrogen source is then passed through in quartz ampoule, nitrogen source is ammonia and nitridation
Magnesium, then carry out carbonization treatment and activation process obtains nitrating activated carbon；Activation process, microwave irradiation work(are carried out with microwave irradiation
Rate is 1000W, and the time of microwave irradiation is 16 minutes.Activation process is carried out simultaneously with carbonization treatment, and carburizing temperature is 1000 DEG C.
(4) above-mentioned nitrating activated carbon is fully washed with watery hydrochloric acid, step (4) nitrating activated carbon concentration is
The salt acid elution that 1.4mol/ rises, wash time are 16 hours, and wash temperature is 65 DEG C, then is repeatedly washed with water, finally dry
To anthracite nitrating activated carbon product.Drying temperature after washing is 110 DEG C, and drying time is more than 10 hours.
Obtained anthracite nitrating activated carbon yield is 47.1%~75.3%.The anthracite nitrating activated carbon of gained is to Asia
For the adsorbance of methyl blue in 340.9mg/g~1233.5mg/g, iodine absorption number is 34.5mg/g~146.8mg/g；Anthracite is mixed
Nitrogen activated carbon BET specific surface area is 779.85m2/ g~1750m2/ g, total pore volume 0.401cm3/ g~0.589cm3/ g, it is average
Aperture is 1-9nm.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
Know the personage of this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Cause
This, all those of ordinary skill in the art without departing from disclosed spirit with being completed under technological thought
All equivalent modifications or change, should by the present invention claim be covered.
Claims (10)
1. a kind of preparation method of anthracite nitrating activated carbon, it is characterised in that comprise the following steps：
(1) anchracite duff for removing impurity is broken into powder first, then dried powder；
(2) dried anthracite powder is transferred in quartz ampoule after being well mixed with activator, anthracite powder and activator
Mass ratio is 1:(1-4)；
(3) nitrogen or inert gas purge quartz ampoule and sample are passed through, nitrogen source is then passed through in quartz ampoule, is then carbonized
Processing and activation process obtain nitrating activated carbon；
(4) above-mentioned nitrating activated carbon is fully washed with watery hydrochloric acid, then repeatedly washed with water, be finally dried to obtain anthracite nitrating
Activated carbon product.
A kind of 2. preparation method of anthracite nitrating activated carbon according to claim 1, it is characterised in that：In step (1)
Its particle diameter is less than 800 microns after anthracite powder crushes, and drying temperature is 80-120 DEG C, and drying time is 8-15 hours.
A kind of 3. preparation method of anthracite nitrating activated carbon according to claim 1, it is characterised in that：Step (2)
Activator includes at least one of potassium hydroxide, zinc chloride, iron chloride, sodium hydroxide.
A kind of 4. preparation method of anthracite nitrating activated carbon according to claim 1, it is characterised in that：Step (2) nothing
Bituminous coal powder adds water during being mixed with activator and obtains the mass ratio 1 of slurry, wherein activator and water:1, obtain
Slurry, which evaporates 3-6 hours in 60 DEG C, is gone out most of moisture, then slurry is dried 24 hours in 80 DEG C, is then transferred into quartz ampoule
In.
A kind of 5. preparation method of anthracite nitrating activated carbon according to claim 1, it is characterised in that：Step (3) makes
Nitrogen source is ammonia, magnesium nitride at least one.
A kind of 6. preparation method of anthracite nitrating activated carbon according to claim 1, it is characterised in that：Step (3) is used
Microwave irradiation carries out activation process, and microwave irradiation power is 400-1200W, and the time of microwave irradiation is 6-20 minutes.
A kind of 7. preparation method of anthracite nitrating activated carbon according to claim 1, it is characterised in that：Step (3) is living
Change processing to carry out simultaneously with carbonization treatment, carburizing temperature is 500-1200 DEG C.
A kind of 8. preparation method of anthracite nitrating activated carbon according to claim 1, it is characterised in that：Step (4) is mixed
Nitrogen activated carbon concentration is the salt acid elution that 0.8-1.6mol/ rises, and wash time is 10-20 hours, wash temperature 50-70
DEG C, then repeatedly washed with water, the drying temperature after washing is 70-120 DEG C, and drying time is more than 10 hours.
9. the anthracite nitrating activated carbon that preparation method described in a kind of claim 1 to 8 any one obtains.
10. anthracite nitrating activated carbon according to claim 9, it is characterised in that：The anthracite nitrating activated carbon of gained
To the adsorbance of methylene blue in 340.9mg/g~1233.5mg/g, iodine absorption number is 34.5mg/g~146.8mg/g；Smokelessly
Coal nitrating activated carbon BET specific surface area is 779.85m2/ g~1750m2/ g, total pore volume 0.401cm3/ g~0.589cm3/ g,
Average pore size is 1-9nm.
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| CN109835897A (en) * | 2019-04-02 | 2019-06-04 | 四川轻化工大学 | Metal/heteroatom modified distiller's grain-based activated carbon and preparation method thereof |
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| CN110182799A (en) * | 2019-06-18 | 2019-08-30 | 咸阳职业技术学院 | It is a kind of to manufacture nitrogenous active carbon and its manufacturing method with anthracite |
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Application publication date: 20180109 |