CN106115698B - A kind of method for preparing nitrogenous porous charcoal using the useless charcoal of recycling and products thereof and application - Google Patents
A kind of method for preparing nitrogenous porous charcoal using the useless charcoal of recycling and products thereof and application Download PDFInfo
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- CN106115698B CN106115698B CN201610487519.6A CN201610487519A CN106115698B CN 106115698 B CN106115698 B CN 106115698B CN 201610487519 A CN201610487519 A CN 201610487519A CN 106115698 B CN106115698 B CN 106115698B
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/006—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by hydrogenation of aromatic hydroxy compounds
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- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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Abstract
The invention discloses a kind of method for preparing nitrogenous porous charcoal using the useless charcoal of recycling, using waste active carbon as raw material, after being mixed with composite activating agent, heating and calcining, calcined product is mixed with deionized water, staticly settled, and sediment is obtained by filtration, then post-treated obtains the nitrogenous porous charcoal；The composite activating agent includes component A and component B, and component A is sodium acid carbonate, and component B is nitrogenous compound.The present invention provides a kind of method for the nitrogenous porous carbon material for obtaining functionalization to waste active carbon progress activating and regenerating using composite activating agent, the recycling to activator is also realized in this method at the same time, greatly reduces cost recovery.The preparation method is simple to operation, existing activated carbon generation technique can directly be utilized, and the Carbon Materials that recycling obtains not only there is abundant absorption property can be used in waste water from dyestuff, moreover it is possible to prepares high performance catalyst as catalyst carrier, greatly improves the added value of waste active carbon.
Description
Technical field
The invention belongs to waste active carbon recycling field, is specifically related to a kind of useless charcoal of utilization recycling and prepares nitrogenous porous charcoal
Method and products thereof and application.
Background technology
Activated carbon has larger specific surface area and flourishing gap, is common absorption in daily life and industrial production
Agent.In daily life, activated carbon is generally used for the pernicious gas of absorption or the purification for drinking water.Led in commercial Application
Domain, activated carbon all play a significant role in many process conditions, are mainly used for the purification of pernicious gas, the decoloration of product and remove
It is smelly.In use, activated carbon can lose adsorption capacity due to adsorption saturation, be abandoned generally as discarded object, burn
Burn or carry out landfill disposal.
Directly from activated carbon precursor, such as biomass or petroleum industry product, prepare activated carbon generally to undergo carbonization and
Two steps are activated, its preparation process is cumbersome, and production cost is high.Directly if functionalization can be prepared from discarded activated carbon
Activated carbon, be on the one hand capable of the absorption property of activity recovery charcoal, on the other hand activated carbon changed during regenerated
Performance enough assigns regenerated activated carbon other functions, is such as used as catalyst carrier.
Researcher mainly passes through thermal regeneration method, chemical reagent method of reproduction, bio-regeneration method, electrochemical regeneration method and micro-
The methods of wave radiation method of reproduction, carries out the regeneration of discarded activated carbon.Since chemical activation method recycles with being lived discarded activated carbon
Property charcoal production process there is similar workshop section to operate, it is not necessary to carry out the improvement of technique, therefore its regeneration cost is relatively low,
Using also than wide.
In chemical activation method, the cost of the activating and regenerating of waste active carbon and the performance of regeneration Carbon Materials depend on work
The selection of agent and technique.At present, it is industrially most of to use steam activation, KOH and ZnCl2Deng activator, vapor is lived
It is bigger to change desired higher (>=1000 DEG C) energy consumptions of temperature, and KOH and ZnCl2Corrosion to consersion unit is larger and it is urged
Agent cannot recycle, therefore production cost is higher.
The content of the invention
The nitrogenous of functionalization is obtained to waste active carbon progress activating and regenerating using composite activating agent the present invention provides a kind of
The method of porous carbon material, the recycling to activator is also realized in this method, greatly reduces cost recovery at the same time.The preparation
Method is simple to operation, can directly utilize existing activated carbon generation technique, and the Carbon Materials that recycling obtains are not only with rich
Rich absorption property can be used in waste water from dyestuff, moreover it is possible to prepares high performance catalyst as catalyst carrier, is greatly lifted
The added value of waste active carbon.
The invention discloses a kind of method for preparing nitrogenous porous charcoal using the useless charcoal of recycling, including：
Using waste active carbon as raw material, after being mixed with composite activating agent, heating and calcining, calcined product mixes with deionized water,
Staticly settle, sediment is obtained by filtration, then post-treated obtain the nitrogenous porous charcoal；
The composite activating agent includes component A and component B, and component A is sodium acid carbonate, and component B is nitrogenous compound.
The present invention using waste active carbon as raw material, waste active carbon because being filled so as to losing adsorption activity by adsorbate in its duct,
And adsorbate is largely some organic molecules, it is in high-temperature burning process since the catalytic action of activator can divide rapidly
Solution, so as to discharge original duct so that waste active carbon recovers adsorption capacity.The present invention is used by sodium acid carbonate and nitrogenous first
The composite activating agent of compound composition, sodium acid carbonate can first decompose generation sodium carbonate in calcination process, and sodium carbonate is at high temperature
It can react with charcoal, Carbon Materials are performed etching, produce duct；And nitrogenous compound can decompose generation in calcination process
Nitrogen-containing molecules, such as ammonia, can react so as to fulfill N doping with charcoal.It is thereby achieved that recovering the suction of waste active carbon
N doping is carried out to activated carbon while attached performance.
Preferably, the nitrogenous compound includes at least one in ammonium oxalate, ammonium hydrogen carbonate, urea, melamine
Kind.
Preferably, the mass ratio of component A and component B is 0.25~4 in the composite activating agent:1, more preferably
0.5~2:1.Nitrogenous compound decomposes in heating process produces CO2、CO、H2O、NH3, these gases can activated carbon at high temperature
Material, and NH therein3N atoms can be adulterated.But since the gas of generation can be spread out quickly, its activation capacity
It is limited.The nitrogen content of doping will not be significantly improved with the increase of nitrogenous compound, therefore component A and group in composite activating agent
The suitable mass-energy densities of B are divided effectively to control activating cost under the conditions of obtaining good activation and mixing N.
Preferably, the waste active carbon and the mass ratio of composite activating agent are 1:2~16, more preferably 1:4
~12.The ratio of composite activating agent and waste active carbon can effectively regulate and control the specific surface area of product Carbon Materials and the yield of activation.
Composite activating agent increases, and specific surface area can increase but yield can reduce, but specific surface area will not be with composite activating agent
Increase and it is linearly increasing.Conversely, composite activating agent is reduced, the yield of charcoal can increase but specific surface area can reduce.
Further preferably, the composite activating agent is sodium acid carbonate/ammonium oxalate, and the mass ratio of sodium acid carbonate and ammonium oxalate is 1:
1；The mass ratio of waste active carbon and sodium acid carbonate/ammonium oxalate is 1:8.Using sodium acid carbonate/ammonium oxalate as composite activating agent, this is compound
The decomposition temperature of activator can match with the activation temperature of waste active carbon, and then activation and N doping is better achieved；By
The ratio of optimization, composite activating agent and waste active carbon is 8:Larger specific surface area (1476m can be obtained when 12/ g) and close
Suitable Carbon yield (60%).
Preferably, the source of the waste active carbon is taken off including pharmaceuticals industry decolorization with activated carbon, sugar manufacturing industry
Color processing is with activated carbon, greasy dirt adsorption treatment with activated carbon or air purification processing activated carbon.
Preferably, the temperature of the heating and calcining is 600~1000 DEG C, soaking time is 1~360min；It is further excellent
Choosing, the heating rate of the heating and calcining is 1~15 DEG C/min.Further preferably, the heating and calcining process, with 15 DEG C/min's
Heating rate is warming up to 900 DEG C, and keeps the temperature 1h.
Preferably, the post processing includes washing, drying.Further preferably, the temperature of the drying is 40~120
℃。
Preferably, the filtrate being obtained by filtration is used to absorb the exhaust gas produced in calcination process, through crystallization after adsorption saturation
Component A in processing recycling composite activating agent.
Calcined product is through washing, wherein soluble inorganic salts (mainly sodium carbonate) can be dissolved in water, it is filtered
Gained filtrate is aqueous sodium carbonate afterwards.Sodium carbonate liquor can absorb the carbon dioxide produced in calcination process so as to form carbon
Sour hydrogen sodium solution, sodium acid carbonate is can obtain after crystallization, realizes the recycling of component A in activator.
Therefore, the recycling of activator is also achieved in the present invention, the recycling of waste active carbon can be greatly reduced
Utilize cost.
The invention also discloses the nitrogenous porous charcoal according to above-mentioned method preparation, which has flourishing multi-stage porous
Structure, the surface of functionalization, therefore there is excellent absorption property, catalyst carrier can be used as, or as adsorbent.
Preferably, when the nitrogenous porous charcoal is prepared in hexamethylene reactive ketone for phenol hydrogenation, with described nitrogenous
Porous charcoal is carrier, using palladium as active component.
Preferably, when the nitrogenous porous charcoal is as absorption of the adsorbent for waste water from dyestuff, it is possible to achieve to first
Effective suction of base indigo plant, alizarin yellow, methyl orange, methylene blue, calcein, eight kinds of amino black 10B, peacock green and rose-red dyestuffs
It is attached.Further preferably, the nitrogenous porous charcoal is more suitable for the absorption to malachite green dye waste water.
Compared with prior art, the invention has the advantages that：
(1) present invention, using special composite activating agent, realizes one-step method and nitrogen is prepared using waste active carbon as raw material
The porous charcoal of doping；
(2) preparation method is utilized, the component A in composite activating agent can realize recycling, and component B is used to contain as nitrogen source
The preparation of nitrogen porous charcoal, greatly reduces the cost recovery of activator；
(3) porous charcoal for the N doping being prepared can be simple as the catalyst carrier of functionalization, method；
In conclusion the preparation method mild condition, of low cost, sustainability is strong, it can be achieved that large-scale production.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph (SEM) of nitrogenous porous carbon material prepared by embodiment 1；
Fig. 2 is the transmission electron microscope picture (TEM) of nitrogenous porous carbon material prepared by embodiment 1；
Fig. 3 is the nitrogen adsorption desorption curve (a) of nitrogenous porous carbon material prepared by embodiment 1, and provides waste active carbon
Nitrogen adsorption desorption curve (b) as a comparison；
Fig. 4 is the pore size distribution curve (a) of nitrogenous porous carbon material prepared by embodiment 1, and provides the hole of waste active carbon
Footpath distribution curve (b) is as a comparison；
Fig. 5 be the nitrogenous porous carbon material prepared using embodiment 1 as the transmission electron microscope picture after carrier loaded palladium, and on carrier
The particle diameter distribution of palladium particle；
Fig. 6 be embodiment 1 in as raw material waste active carbon scanning electron microscope (SEM) photograph (SEM)；
Fig. 7 is the scanning electron microscope (SEM) photograph (SEM) of nitrogenous porous carbon material prepared by embodiment 2；
Fig. 8 is that nitrogenous porous carbon material prepared by embodiment 1 is yellow to methyl blue, alizarin yellow, methyl orange, methylene blue, calcium
The absorption property of green element, amino black 10B, peacock green and eight kinds of dyestuffs of rose-red.
Embodiment
Following embodiment will more comprehensively describe the present invention.
Embodiment 1：The useless charcoal produced using decolorization in biotin generating process is raw material.
2g waste active carbons, 8g sodium acid carbonates and 8g ammonium oxalate are weighed, is transferred to after mechanical mixture in 30ml crucibles, then
Calcined in nitrogen furnace.The step of calcining is：900 DEG C are warming up to 15 DEG C/min, 1h is calcined at 900 DEG C；Then it is natural
Cool to room temperature.Product after calcining is polished to be mixed with deionized water, is filtered after standing 24h, sediment is again through washing
Wash to neutrality, drying and obtain the nitrogenous porous carbon material.
The scanning electron microscope (SEM) photograph and transmission electron microscope picture of nitrogenous porous carbon material manufactured in the present embodiment are as shown in Figure 1, 2：
Observe Fig. 1 and understand that the charcoal material surface after activation contains some ducts, its microcellular structure can be observed by Fig. 2.
Nitrogen adsorption desorption curve and the hole of nitrogenous porous carbon material manufactured in the present embodiment are provided in Fig. 3 and Fig. 4 respectively
Footpath distribution curve, and provide the waste active carbon as raw material nitrogen adsorption desorption curve and pore size distribution curve as a comparison.
Observe two figures and understand that nitrogenous porous carbon material manufactured in the present embodiment has larger specific surface area, while includes micropore and Jie
Hole.And most of pore passage structure of waste active carbon as a comparison is all filled, adsorption activity is lost.Fig. 6 is the waste active carbon
Scanning electron microscope (SEM) photograph, also support above-mentioned conclusion.
The element group in the product prepared in embodiment 1 as the useless porous charcoal of raw material with embodiment 1 is listed in table 1
Into.
Table 1
A is the waste active carbon as raw material in embodiment 1；
B is nitrogenous porous charcoal prepared by embodiment 1.
As shown in Table 1, after composite activating agent activates, the nitrogen content in product increases to 3%.
Application examples 1：Prepared using nitrogenous porous charcoal prepared by embodiment 1 as carrier loaded palladium and prepare hexamethylene for phenol hydrogenation
The catalyst of ketone
The nitrogenous porous charcoal (NAC) that embodiment 1 is prepared utilizes the side of ultrasonic assistant soakage and sodium borohydride reduction
Method, has been prepared the catalyst that palladium load capacity is 5wt%.
Fig. 5 is the nitrogenous porous charcoal using the preparation of embodiment 1 as the transmission electron microscope after catalyst carrier supported palladium (5wt%)
Figure.As seen from the figure, the average grain diameter of palladium particle is 3.3nm.
The catalyst of above-mentioned preparation is prepared in the reaction of cyclohexanone for phenol hydrogenation, each raw material dosage, reaction condition
And catalytic result is shown in Table 2.
Table 2
As shown in Table 2, the nitrogenous porous charcoal that prepared by embodiment 1 can prepare ring as carrier loaded palladium chtalyst phenol hydrogenation
Hexanone, and there is very high activity and selectivity.
Application examples 2：Waste water from dyestuff is adsorbed using nitrogenous porous charcoal prepared by embodiment 1 as adsorbent
Respectively with methyl blue, alizarin yellow, methyl orange, methylene blue, calcein, amino black 10B, peacock green and rose-red
Eight kinds of dyestuffs is deal with objects, the absorption property of nitrogenous porous charcoal prepared by testing example 1.Specific operating process is as follows：
Take nitrogenous porous charcoal prepared by 10mg embodiments 1 to be added in the aqueous dye solutions of 20ml 1M, stirred under room temperature
24h reaches saturation absorption, is tested using uv-vis spectra, test result is as shown in Figure 8.
Observe Fig. 8 to understand, the nitrogenous porous charcoal prepared through the present invention has good absorption property to most of dyestuff, especially
It is that have excellent absorption property to peacock green.
Embodiment 2：Waste active carbon after being decolourized using sugar industry is raw material
Weigh 2g waste active carbons and carry out mechanical mixture with the potassium oxalate of 8g sodium acid carbonates and 8g, be then transferred into 30ml crucibles
In.Then calcined again in nitrogen furnace.The step of calcining is to be warming up to 900 DEG C with 15 DEG C/min, and 1h is calcined at 900 DEG C；So
Temperature fall is to room temperature afterwards.Mixture grinding after calcining is broken, then washed using 300ml deionized waters into every trade, after 24h
Filtered, be washed till neutrality, drying obtains nitrogenous porous carbon material.Its scanning electron microscope (SEM) photograph (SEM) is as shown in Figure 7.
Claims (3)
- A kind of 1. method for preparing nitrogenous porous charcoal using the useless charcoal of recycling, it is characterised in that including：Using waste active carbon as raw material, after being mixed with composite activating agent, heating and calcining, calcined product is mixed with deionized water, stood Precipitation, is obtained by filtration sediment, then post-treated obtains the nitrogenous porous charcoal；The filtrate being obtained by filtration, which is used to absorb, calcines During the exhaust gas that produces, recycle the component A in composite activating agent through crystallization treatment after adsorption saturation；The composite activating agent includes component A and component B, and component A is sodium acid carbonate, and component B is nitrogenous compound；The nitrogenous compound includes at least one of ammonium oxalate, urea, melamine；The mass ratio of component A and component B is 0.25~4 in the composite activating agent:1；The mass ratio of the waste active carbon and composite activating agent is 1:2~16.
- 2. the method according to claim 1 for preparing nitrogenous porous charcoal using the useless charcoal of recycling, it is characterised in that described answers Conjunction activator is sodium acid carbonate/ammonium oxalate, and the mass ratio of sodium acid carbonate and ammonium oxalate is 1:1；The mass ratio of the waste active carbon and sodium acid carbonate/ammonium oxalate is 1:8.
- 3. the method according to claim 1 for preparing nitrogenous porous charcoal using the useless charcoal of recycling, it is characterised in that the heating The temperature of calcining is 600~1000 DEG C, and soaking time is 1~360min.
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| CN107902655A (en) * | 2017-11-24 | 2018-04-13 | 浙江工业大学 | A kind of method for preparing nitrating activated carbon using discarded activated carbon |
| CN111689496A (en) * | 2019-03-12 | 2020-09-22 | 淮阴师范学院 | Persimmon peel-based nitrogen-doped activated carbon and preparation method thereof |
| CN110075798A (en) * | 2019-05-07 | 2019-08-02 | 安徽工大化工科技有限公司 | It is a kind of for handling the preparation method of the biomass adsorbent of metal ion waste water |
| CN110075800A (en) * | 2019-05-07 | 2019-08-02 | 安徽工大化工科技有限公司 | A kind of biomass adsorbent |
| CN111298847B (en) * | 2020-03-03 | 2021-05-04 | 清华大学 | Method for regenerating carbon-based catalyst, carbon-based catalyst and water treatment method |
| CN113000041B (en) * | 2021-02-26 | 2023-03-28 | 上海大学材料基因组工程(萍乡)研究院 | Regeneration method of waste activated carbon by using biomass |
| CN113683090A (en) * | 2021-09-23 | 2021-11-23 | 湖南省格林森炭业股份有限公司 | Activated carbon multi-element composite activating agent |
| CN114956074A (en) * | 2022-06-17 | 2022-08-30 | 西安交通大学 | Seaweed-based three-dimensional porous carbon sieve and preparation method thereof |
| CN114950578A (en) * | 2022-07-05 | 2022-08-30 | 江苏治水有数环保科技有限公司 | Catalyst regeneration process |
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| CN102698724A (en) * | 2012-04-06 | 2012-10-03 | 淮北市大华活性炭有限公司 | Method for producing active carbon for gasoline vapor adsorption |
| CN104447209A (en) * | 2014-11-19 | 2015-03-25 | 浙江大学 | Method for preparing cyclohexanol by catalyzing by base metal catalyst |
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| CN102698724A (en) * | 2012-04-06 | 2012-10-03 | 淮北市大华活性炭有限公司 | Method for producing active carbon for gasoline vapor adsorption |
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