CN105692611B - A kind of preparation method of the activated carbon from activated sludge rich in nitrogen and oxygen - Google Patents
A kind of preparation method of the activated carbon from activated sludge rich in nitrogen and oxygen Download PDFInfo
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- CN105692611B CN105692611B CN201610161961.XA CN201610161961A CN105692611B CN 105692611 B CN105692611 B CN 105692611B CN 201610161961 A CN201610161961 A CN 201610161961A CN 105692611 B CN105692611 B CN 105692611B
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Abstract
The invention belongs to specific function absorbent charcoal material technical field.The invention provides a kind of preparation method of the activated carbon from activated sludge rich in nitrogen and oxygen, concretely comprise the following steps：A certain amount of biomass material is added in the solution of nitrogenous thing and alkaline matter; all substances are moved into hydrothermal reaction kettle afterwards; reaction a period of time at a certain temperature; reaction naturally cools to room temperature after terminating; product is taken out into drying; by dried product, the high temperature cabonization under protective gas atmosphere activates certain time in high temperature process furnances again, and reaction terminates rear natural cooling, biomass active product char of the drying to obtain rich in nitrogen after product is washed repeatedly.Using the biomass active carbon rich in nitrogen and oxygen prepared by this method due to introducing nitrogen, oxygen heteroatom so as to improving wellability of the carbon material to water in itself and the absorption property to electrolyte ion, it can be widely applied to pollutant process, the separation of mixture and electrode material etc., are with a wide range of applications.
Description
Technical field
The invention belongs to specific function absorbent charcoal material technical field, and in particular to a kind of biomass rich in nitrogen and oxygen is lived
The manufacture method of property charcoal.
Background technology
Activated carbon rich in nitrogen, oxygen is that a part of carbon atom is substituted by nitrogen-atoms and oxygen atom in carbon structure, thus is had
There is the surface chemical property of uniqueness, the relatively unazotized activated carbon of activated carbon rich in nitrogen, oxygen has more preferable hydrophily and suction
Attached ability, there is higher absorption property to sulphur system and compound nitrogen series, simultaneously because nitrogen-atoms, oxygen atom electronic shell delocalization energy
Power is stronger thus has higher chemical property.Prepare at present nitrogenous, oxygen-content active charcoal common preparation method have template,
Method of carbonization/activation nitrogenous precursor etc..Wherein most important research is that different works are studied using nitrogenous precursor as raw material
The influence of skill.
A kind of entitled patents of the preparation method of nitrogenous activated-carbon catalyst of patent CN102553641B, will be carbonized
Material is impregnated with strong oxidizer or reflow treatment, is blended afterwards with nitrogenous reagent with certain proportion, moves into high temperature process furnances in inertia
Activated under atmosphere, prepare the activated carbon product rich in nitrogen.Patent CN102360959A utilizes the ureaformaldehyde tree rich in nitrogen
Fat makees raw material, charing, work of the activation preparation rich in nitrogen after being blended after raw material is carbonized under an inert atmosphere with potassium hydroxide
Property charcoal.Patent CN103408007A is added in ethanol solution using normal activated carbon or carbon material, is added melamine and is discarded
Thing blending and stirring is ultrasonically treated, and carbonization-activation is handled under inert atmosphere in high temperature furnace afterwards, prepares nitrogenous activated carbon.Patent
CN104681307A is carried out activation with phosphoric acid after being carbonized using the discarded particieboard rich in Lauxite and is prepared for being rich in nitrogen
With the activated carbon of oxygen element.But the above method has either only introduced nitrogen heteroatom or has taken different step to introduce nitrogen respectively
Atom and oxygen atom, technique is cumbersome, is unfavorable for industrialized production.Increased simultaneously in activated carbon using hydro-thermal reaction nitrogen and
The research of the activated carbon from activated sludge of oxygen element content is also without open report.
The content of the invention
For prior art problem, the present invention utilizes hydro-thermal reaction method, there is provided a kind of biomass active rich in nitrogen and oxygen
The preparation method of charcoal.
Technical scheme is as follows：
The preparation method of the activated carbon from activated sludge rich in nitrogen and oxygen of the present invention, comprises the following steps：
1) a certain amount of biomass material is added in the mixed solution of certain density nitrogen substance and alkaline matter,
All substances are subjected to hydro-thermal reaction for a period of time at a certain temperature afterwards, reaction naturally cools to room temperature after terminating；
2) product of step 1) is taken out into drying, then dried product high temperature cabonization is activated into certain time, reaction knot
Natural cooling after beam；
3) activated carbon from activated sludge of the drying to obtain rich in nitrogen and oxygen after the product washing after step 2) carbonization-activation is produced
Thing.
Preparation in accordance with the present invention, wherein, described biomass material includes forestry rubbish, agricultural crop straw, fruit
One or more in real shell, crudefiber crop or other plant stem-leafs.Particularly preferably, described forestry rubbish can include timber
One or more in leftover pieces, sawdust and particieboard；The agricultural crop straw can include wheat stalk, maize straw, water
One or more in rice straw and broomcorn straw；The fruit shell can include walnut shell, Pericarppium Armeniacae Amarum, peanut shell, coconut
One or more in shell and pine nut shell；The crudefiber crop can be one or two kind in sisal hemp and hemp.
Preparation in accordance with the present invention, wherein, described nitrogen substance include ammoniacal liquor, hydrazine water, ammonium carbonate, ammonium sulfate and
One or more in urea.Preferably, the mass fraction of the nitrogen substance in the mixed solution is in 10%-30%.
Preparation in accordance with the present invention, wherein, described alkaline matter include potassium hydroxide, sodium hydroxide, potassium carbonate,
One or more in sodium carbonate.Preferably, the mass fraction 2%-20% of the alkaline matter in the mixed solution.
Preparation in accordance with the present invention, wherein, the mixing of described biomass material and nitrogen substance and alkaline matter
The mass ratio of solution is 1：5~1：20.
Preparation in accordance with the present invention, wherein, the hydrothermal temperature described in step 1) is 180-240 DEG C, the water
The time of thermal response is 1-6 hours.
Preparation in accordance with the present invention, wherein, the high temperature cabonization activation temperature described in step 2) is 500-900 DEG C, high
The warm carbonization-activation time is -3 hours 30 minutes.Preferably, step 2) the high temperature cabonization activation is in high temperature process furnances
Carry out, the protective gas described in step 2) is the one or more of nitrogen, helium, neon, argon gas, Krypton, xenon and radon gas.
The present invention technical characterstic be：Innovative agent of mixing nitrogen adds hydrothermal reaction process, by and nitrogenous reagent
Reaction introduce nitrogen-containing group on raw material, and hydrothermal reaction process, water not only aoxidize as a kind of again as a kind of reaction dissolvent
Agent, raw material is set to be grafted the oxy radical enriched.The biomass active carbon for being rich in nitrogen, oxygen prepared using this method is due to introducing
Nitrogen, oxygen heteroatom can be widely applied to so as to improve its wellability to water and the absorption property to electrolyte ion
Pollutant process, the separation of mixture and electrode material etc., is with a wide range of applications.
Brief description of the drawings
Fig. 1 is the optical photograph of intermediate when being prepared rich in nitrogen and oxygen element wheat husk activated carbon of the present invention.
Fig. 2 is the optical photograph rich in nitrogen and oxygen element wheat husk activated carbon of the present invention.
Embodiment
With reference to specific embodiment, the invention will be further described.
Embodiment 1
By 10g wheat husks, mixing of the 100g containing the ammoniacal liquor of mass fraction 10% and potassium hydroxide that mass fraction is 5% is added to
In solution, fully moved into after infiltration in hydrothermal reaction kettle, hydro-thermal reaction is carried out under 240 degree 2 hours, reaction is cooled to after terminating
Room temperature, product is filtered and takes out drying, as shown in figure 1, dried product is put into high temperature process furnances, at 600 degrees Celsius
The lower reaction of nitrogen protection 0.5 hour.After reaction terminates, room temperature is down to, product is taken out, is cleaned repeatedly with deionized water, dried
The sisal hemp NACF rich in nitrogen and oxygen is obtained afterwards.As shown in Figure 2.
Embodiment 2
By 3g corncobs, mixing of the 60g containing the ammoniacal liquor of mass fraction 30% and potassium carbonate that mass fraction is 10% is added to
In solution, fully moved into after infiltration in hydrothermal reaction kettle, hydro-thermal reaction is carried out under 180 degree 6 hours, reaction is cooled to after terminating
Room temperature, product filtering is taken out after drying, be put into high temperature process furnances, reacted 2 hours in the case where 600 degrees Celsius of nitrogen are protected.Instead
After should terminating, room temperature is down to, product is taken out, is cleaned repeatedly with deionized water, the corn rich in nitrogen and oxygen is obtained after drying
Core activated carbon.
Embodiment 3
By 10g bamboos, mixing of the 50g containing the ammoniacal liquor of mass fraction 20% and potassium hydroxide that mass fraction is 15% is added to
In solution, fully moved into after infiltration in hydrothermal reaction kettle, hydro-thermal reaction is carried out under 220 degree 4 hours, reaction is cooled to after terminating
Room temperature, product filtering is taken out after drying, be put into high temperature process furnances, reacted 1 hour in the case where 800 degrees Celsius of nitrogen are protected.Instead
After should terminating, room temperature is down to, product is taken out, is cleaned repeatedly with deionized water, the bamboo rich in nitrogen and oxygen is obtained after drying and is lived
Property charcoal.
Embodiment 4
By 5g sawdusts, 100g is added to containing the potassium hydroxide and quality of the hydrazine water of mass fraction 20% and mass fraction for 5%
In mixed solution of the fraction for the potassium carbonate of 2% content, fully moved into after infiltration in hydrothermal reaction kettle, enter water-filling under 200 degree
Thermal response 2 hours, reaction are cooled to room temperature after terminating, and product filtering are taken out after drying, are put into high temperature process furnances, 900
The lower reaction of degree Celsius nitrogen protection 0.5 hour.After reaction terminates, room temperature is down to, product is taken out, it is repeatedly clear with deionized water
Wash, the bamboo absorbent charcoal rich in nitrogen and oxygen is obtained after drying.
Embodiment 5
By 5g walnut shells, it is 15% potassium hydroxide to be added to 50g containing the ammonium carbonate of mass fraction 10% and mass fraction
In mixed solution, fully moved into after infiltration in hydrothermal reaction kettle, hydro-thermal reaction is carried out under 220 degree 3 hours, reaction terminates rear cold
But to room temperature, product filtering is taken out after drying, be put into high temperature process furnances, reaction 2 is small in the case where 800 degrees Celsius of nitrogen are protected
When.After reaction terminates, room temperature is down to, product is taken out, is cleaned repeatedly with deionized water, be to obtain rich in nitrogen and oxygen after drying
Bamboo absorbent charcoal.
Embodiment 6
By 10g wheat husks, it is the mixed of 20% sodium hydroxide to be added to 100g containing the urea of mass fraction 10% and mass fraction
Close in solution, fully moved into after infiltration in hydrothermal reaction kettle, hydro-thermal reaction is carried out under 240 degree 1 hour, reaction cools down after terminating
To room temperature, product is filtered and takes out drying, dried product is put into high temperature process furnances, protected in 500 degrees Celsius of nitrogen
Lower reaction 3 hours.After reaction terminates, room temperature is down to, product is taken out, is cleaned repeatedly with deionized water, richness is obtained after drying
The nitrogenous and sisal hemp NACF of oxygen.
Embodiment 7
By 3g corncobs, mixing of the 60g containing the ammonium sulfate of mass fraction 30% and sodium carbonate that mass fraction is 2% is added to
In solution, fully moved into after infiltration in hydrothermal reaction kettle, hydro-thermal reaction is carried out under 200 degree 4 hours, reaction is cooled to after terminating
Room temperature, product filtering is taken out after drying, be put into high temperature process furnances, reacted 1 hour in the case where 700 degrees Celsius of nitrogen are protected.Instead
After should terminating, room temperature is down to, product is taken out, is cleaned repeatedly with deionized water, the corn rich in nitrogen and oxygen is obtained after drying
Core activated carbon.
Certainly, the present invention can also have various embodiments, in the case of without departing substantially from spirit of the invention and its essence, be familiar with
Those skilled in the art can be made according to disclosure of the invention it is various it is corresponding change and modifications, but these it is corresponding change and
Deformation should all belong to the protection domain of appended claims of the invention.
Claims (10)
1. a kind of preparation method of the activated carbon from activated sludge rich in nitrogen and oxygen, comprises the following steps：
1) a certain amount of biomass material is added in the mixed solution of certain density nitrogen substance and alkaline matter, afterwards
All substances are subjected to hydro-thermal reaction for a period of time at a certain temperature, reaction naturally cools to room temperature after terminating；
2) product of step 1) is taken out into drying, then the high temperature cabonization activation one under protective gas atmosphere by dried product
Fix time, reaction terminates rear natural cooling；
3) by biomass active product char of the drying to obtain rich in nitrogen and oxygen after the product washing after step 2) carbonization-activation.
2. preparation method according to claim 1, it is characterised in that described biomass material includes forestry rubbish, agriculture
One or more in crop material, fruit shell, crudefiber crop or other plant stem-leafs.
3. preparation method according to claim 1, it is characterised in that described nitrogen substance includes ammoniacal liquor, hydrazine water, carbonic acid
One or more in ammonium, ammonium sulfate and urea.
4. according to the preparation method described in claims 1, it is characterised in that described biomass material and the matter of mixed solution
Amount is than being 1：5~1：20.
5. according to any described preparation method in claim 1,3 or 4, it is characterised in that the nitrogenous thing in the mixed solution
The mass fraction of matter is in 10%-30%.
6. preparation method according to claim 1, it is characterised in that described alkaline matter includes potassium hydroxide, hydrogen-oxygen
Change the one or more in sodium, potassium carbonate, sodium carbonate.
7. the preparation method according to claim 1 or 6, it is characterised in that the matter of the alkaline matter in the mixed solution
Amount fraction is 2%-20%.
8. preparation method according to claim 1, it is characterised in that the hydrothermal temperature described in step 1) is 180-
240 DEG C, the time of the hydro-thermal reaction is 1-6 hours.
9. preparation method according to claim 1, it is characterised in that the high temperature cabonization activation temperature described in step 2) is
500-900 DEG C, high temperature cabonization soak time is -3 hours 30 minutes.
10. preparation method according to claim 1, it is characterised in that described protective gas is nitrogen, helium, neon
Gas, argon gas, Krypton, the one or more of xenon and radon gas.
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