CN105921109A - Biological carbon prepared from tobacco stems as well as preparation method and application thereof - Google Patents
Biological carbon prepared from tobacco stems as well as preparation method and application thereof Download PDFInfo
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- CN105921109A CN105921109A CN201610382287.8A CN201610382287A CN105921109A CN 105921109 A CN105921109 A CN 105921109A CN 201610382287 A CN201610382287 A CN 201610382287A CN 105921109 A CN105921109 A CN 105921109A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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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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Abstract
The invention discloses a method for preparing biological carbon from tobacco stems. The method for preparing the biological carbon from the tobacco stems comprises the following steps: (1), crushing the tobacco stems, and then enabling the crushed tobacco stems and water to be subjected to a hydrothermal carbonization reaction at 180-260 DEG C; after terminating the reaction, filtering, washing and drying an obtained product in sequence; (2), activating the product, which is dried in Step (1), by an activating agent, afterwards, calcining the activated product at 400-1200 DEG C in an inert atmosphere, and subsequently, washing the calcined product with water, drying the water-washed product, and obtaining the biological carbon. The activating agent is at least one of a lewis acid, a peroxide, an alkali metal hydroxide and an alkali metal carbonate. The invention also discloses the biological carbon prepared by adopting the method and application of the biological carbon to the adsorption of heavy metal. An obtained biological carbon material has advantages of relatively small particle sizes, relatively large specific surface area, relatively strong adsorption capacity and the like, and can be applied to the adsorption and the repair of heavy metal ions in a water body and a soil environment.
Description
Technical field
The present invention relates to agrochemical field, the charcoal that utilizes cabo to prepare particularly to a kind of, system
Preparation Method and application thereof.
Background technology
In recent years, heavy metal pollution situation is the severeest, and especially the pollution in soil and water body is more
Seriously, jeopardizing safety in production and the utilization of grain, the survival and development to the mankind constitute a serious threat.
Utilize biomass raw material to prepare functionalization charcoal to can be used for administering and repairing heavy metal pollution.
China is tobacco leaf production big country, and annual tobacco leaf production amount is about the 42% of the whole world.At home
In economic system, property tax value produced by Nicotiana tabacum L. occupies important dividing in the economic total value in the whole nation
Amount.Cabo is the by-product of tobacco industry, has few hundred thousand tonnes of cabo resource to go out of use every year.And cabo
In content of organics be about 90%-95%, mineral nitrogen, phosphorus, potassium content are about 5%-10%, with
Time possibly together with some trace element, there is compared with other crops the advantage of its uniqueness.Additionally, cigarette
Containing substantial amounts of lignin, cellulose and nicotine in stalk, common bacterial strain is difficult to decompose, it is impossible to just
Also field, ground.How making good use of waste tobacco stem is the difficult problem that tobacco industry needs to solve, and is also that agricultural can be held
One vital task of supervention exhibition.
Charcoal is that biomass (Wastes of Crops, timber, plant tissue, animal skeleton etc.) are in anoxia
Under conditions of, Pintsch process carbonization and the high charcoal of a kind of carbon content of being formed.The specific surface of charcoal
Long-pending and porosity is relatively big, possess stronger absorption affinity, Resistance to microbes ability, resistance to oxidation, this
Charcoal is made to can be widely applied to the fields such as industry, agricultural, the energy, environment.According to mode of heating
Difference, the preparation method of biomass carbon can be divided into thermal decomposition method, microwave charring and hydro-thermal charring.
Hydro-thermal carbonization can accelerate the physics chemical action between biomass and solvent, the carbon water in decomposing biomass
Compound structure, ultimately forms biomass carbon material and separates out.The aqueous medium atmosphere of hydro-thermal carbonization helps
The formation of material surface oxygen-containing functional group in carbonization process, therefore carbonizing production typically contains abundant
The adsorption of surface functional group, beneficially heavy metal ion.Meanwhile, charcoal be a kind of low cost,
High efficiency environmental friendliness shaped material, beneficially industrialized production.
Summary of the invention
It is an object of the invention to provide one and utilize agricultural production refuse cabo simple and quick preparation height
The method of quality charcoal；It addition, the present invention also provide for charcoal that a kind of described method prepares and
It is in the application of Adsorption of Heavy Metals.
A kind of method utilizing cabo to prepare charcoal, comprises the following steps:
Step (1): cabo carries out hydro-thermal carbonization reaction with water after pulverizing at 180 DEG C～260 DEG C；
Reaction sequentially pass through again after terminating filtrations, wash, dry；
Step (2): again at inert atmosphere after the activation of activated dose of step (1) dried product
Calcine at 400 DEG C～1200 DEG C, wash subsequently, be drying to obtain charcoal；Described activator is Louis
At least one in this acid, peroxide, alkali metal hydroxide, alkali carbonate.
In the present invention, the hydro-thermal carbonization process of step (1) and the activator activation processing of step (2)
Mode coordinated, can make cabo discharge aldehydes matter, Benzene and Homologues, generation the least
Molecular compound, the most prepared particle size is less, specific surface area is relatively big, absorbability is stronger
Charcoal.
Cabo particle after pulverizing adds to water (e.g., deionized water), seals extremely pressure reaction and sets
Standby (autoclave) carries out the hydro-thermal carbonization reaction of anaerobic or anoxia.
In the present invention, in step (1), cabo pulverized particles degree, hydro-thermal carbonization reaction temperature are the most right
The performance of the charcoal prepared has an impact.
As preferably, the granularity after cabo is pulverized is 40～100 mesh.Wherein pulverized particles degree is in institute
In the range of stating preferably, the specific surface area of cabo powder is relatively big, can be fully contacted with water in course of reaction,
Make reaction carry out completely as much as possible, the absorption property of obtained charcoal can be improved simultaneously.Such as cabo
The Carbon Materials that pulverized particles degree is obtained under the conditions of 30 mesh is 20mg/g to the water adsorption amount of lead ion
Above, and after further experiment, Carbon Materials obtained under the conditions of cabo pulverized particles degree is 60 mesh
Adsorbance to lead ion is more than 40mg/g.
In step (1), cabo is 1g: 2～15ml with the w/v of water.
Carrying out hydro-thermal reaction at said temperatures, prepared material degree of carbonization is higher, and porosity is relatively big,
Under conditions of being 150 DEG C such as hydro-thermal carbonization temperature, its specific surface area is about 350m2/ g, hydro-thermal carbonization temperature
Under conditions of degree is 180 DEG C, its specific surface area is about 420m2/g。
As preferably, hydro-thermal carbonization temperature is in the range of 180～200 DEG C.
During hydro-thermal carbonization reaction, heating rate is 10～20 DEG C/min.
Insulation reaction after described temperature it is warming up under described heating rate, as preferably, hydro-thermal charcoal
The change response time is 2～16h.
After hydro-thermal carbonization reaction terminates, cool down and filter, use deionized water by Cake Wash to pH
(product of step (1) hydro-thermal reaction is non-activated activity to be dried to obtain unactivated charcoal after neutrality
Charcoal), this charcoal carries out the activation processing of step (2) again, changes the surface of this charcoal further
Structure so that it is there is bigger porosity, pore volume, and then improve its absorption property.
In step (1), being dried under vacuum, the temperature being dried is 60～80 DEG C；When being dried
Between be 8～14h.In the process of vacuum drying of step (1), vacuum is less than 0.1MPa.
The product that step (1) is dried to obtain and the aqueous solution of activator, dipping；Washing subsequently,
Dried calcining under atmosphere of inert gases again, after calcining, washing is to neutral, the most i.e. obtains modified
Charcoal (step (2) process prepare for modified charcoal).
The surface portion of the charcoal of step (1) is aoxidized by activator, is formed such as carboxyl, carbonyl etc.
Oxygen-content active functional group, the increase of these functional groups can improve the adsorptivity of charcoal heavy metal ion
Energy.
In step (2), activator and inventory and calcining heat thereof all can affect prepared biology
The specific surface area performance of charcoal.
Existing alkali metal hydroxide such as KOH, NaOH, LiOH etc. all can apply to the present invention
In；Described lewis acid is preferably non-proton lewis acid.Described peroxide is the most water-soluble
Property peroxide, such as hydrogen peroxide, sodium peroxide etc..
As preferably, described activator is ZnCl2、SnCl2、H3PO4、H2O2, KOH or
K2CO3In at least one.
In the aqueous solution of activator, described activator mole percent is 1mol%～10mol%, lives
During change, the mass ratio of the cabo of step (1) and the aqueous solution of activator is 1: 1～5.
Further preferably, described activator is KOH and/or K2CO3。
In step (2), soak time is 1～10 hour.
After activation processing terminates, then under inert gas shielding, carry out calcination processing, increase its carbonization journey
Degree, under conditions of Pintsch process, it is thus achieved that more small-molecule substances, improves its specific surface area.Calcining
The temperature of process, time, gas flow rate all can affect the structure of obtained biological carbon materials, Jin Erying
Ring its absorption property.
Existing conventional noble gas such as nitrogen, argon etc. all can be as the protective gas of calcination process.
As preferably, calcination process is carried out under nitrogen protection, and wherein, the flow velocity of nitrogen is
0.8～1.1L/min.
The temperature of calcination process is preferably 400～800 DEG C.
In step (2), the heating rate of calcination process is 2～8 DEG C/min.Heating rate is too fast, holds
Easily the structure of Carbon Materials is destroyed.
The charcoal prepared after activation is spherical in shape, and grain diameter is 0.5～10 μm；Specific surface area is
420～1000m2/g.The epigranular of this charcoal, specific surface area is big, high adsorption capacity.
Present invention additionally comprises the application of a kind of described charcoal Adsorption of Heavy Metals, by described charcoal with
Sample solution contact containing heavy metal.
As, the charcoal using the present invention to prepare mixes containing the water sample of heavy metal, pedotheque with suspecting
Close, the heavy metal in stirring and adsorbing sample.
Adsorption process is for example: hydro-thermal charcoal cabo hydro-thermal carbonization prepared is activated, calcine, wash,
With four kinds of concentration be after drying 10～1000ppm heavy metal ion solution by solid-to-liquid ratio be
The ratio mixing of 0.01g～0.50g: 5～50ml, vibrate 24h, utilizes atomic absorption spectrophotometer to survey
Heavy metal ion solution concentration after fixed absorption.
Obtain charcoal Carbon Materials (charcoal after activation) prepared by employing the inventive method and have less
Particle size, bigger specific surface area, the advantage (particle size: 0.5～10 such as stronger absorbability
μm, specific surface area is 420～1000m2/ g, is 60～70mg/g to cupric ion adsorption).Can answer
For water body and the reparation of Mobility of Heavy Metals In Soil Environment ion.The method utilizes agricultural production garbage,
Prepare charcoal adsorbent by simple and quick hydro-thermal charing method, turn waste into wealth, make full use of money
Source, reduces environmental pollution, good in economic efficiency, develops new technique, is of value to industrialized production.
Accompanying drawing explanation
Fig. 1 is biological carbon materials (sample one) the SEM figure that embodiment 1 prepares；
Fig. 2 is biological carbon materials (sample two) the SEM figure that embodiment 2 prepares；
Fig. 3 is biological carbon materials (sample three) the SEM figure that embodiment 3 prepares；
Fig. 4 is biological carbon materials (sample four) the SEM figure that embodiment 4 prepares；
Fig. 5 is biological carbon materials (sample five) the SEM figure that embodiment 5 prepares；
Fig. 6 is biological carbon materials (sample six) the SEM figure that embodiment 6 prepares；
Fig. 7 is biological carbon materials (sample seven) the SEM figure that embodiment 7 prepares；
Fig. 8 is biological carbon materials (sample eight) the SEM figure that embodiment 8 prepares.
Detailed description of the invention
Following example are pressed aforesaid operations method and are implemented:
Below will by embodiment, the invention will be further described, these describe be not intended to this
The content of invention is further limited.It should be understood by those skilled in the art that present invention
The equivalent that technical characteristic is done, or be correspondingly improved, within still falling within protection scope of the present invention.
Embodiment 1:
Tobacco stem waste after crushed, chooses the granule of 60 mesh, is 1g: 12ml according to solid-to-liquid ratio
After 5g cabo (granule) biomass and 60ml deionized water are stirred by ratio, it is encapsulated into high pressure anti-
Answer in still, under conditions of electric furnace heating rate is 10～20 DEG C/min, carry out hydro-thermal in 180 DEG C
Carbonization 5h, uses deionized water wash to neutrality, sucking filtration, is dried 10h at 70 DEG C after natural cooling
After, grind and obtain cabo biological carbon materials.To obtain cabo charcoal uses KOH activator water-soluble
Liquid (KOH mole percent is 5mol%) mixes postactivated 2h with 1: 4 (solid-liquid weight ratio) ratio,
Dried calcine 2h at 400 DEG C the most under nitrogen protection, clean to neutral with deionized water after natural cooling,
I.e. obtain charcoal after drying.The charcoal SEM figure prepared is shown in Fig. 1.
The particle size of obtained charcoal is 0.5 μm, and specific surface area is 620m2/g。
Embodiment 2:
Tobacco stem waste after crushed, chooses the granule of 60 mesh, is 1g: 12ml according to solid-to-liquid ratio
After 5g cabo biomass and 60ml deionized water are stirred by ratio, it is encapsulated in autoclave
, under conditions of electric furnace heating rate is 10～20 DEG C/min, carry out hydro-thermal carbonization 5h in 180 DEG C,
Use deionized water wash to neutrality, sucking filtration after natural cooling, after being dried 10h at 70 DEG C, grind
Obtain cabo biological carbon materials.Cabo charcoal will be obtained and use K2CO3Activator aqueous solution (K2CO3
Mole percent is 5mol%) mix postactivated 2h, after drying with 1: 4 ratio (solid-liquid weight ratio)
Calcine 2h under nitrogen protection at 400 DEG C, clean to neutral with deionized water after natural cooling, be dried
After i.e. obtain charcoal.The charcoal SEM figure prepared is shown in Fig. 2.
The particle size of obtained charcoal is 0.6 μm, and specific surface area is 600m2/g。
Embodiment 3:
Tobacco stem waste after crushed, chooses the granule of 60 mesh, is 1g: 12ml according to solid-to-liquid ratio
After 5g cabo biomass and 60ml deionized water are stirred by ratio, it is encapsulated in autoclave
, under conditions of electric furnace heating rate is 10～20 DEG C/min, carry out hydro-thermal carbonization 5h in 180 DEG C,
Use deionized water wash to neutrality, sucking filtration after natural cooling, after being dried 10h at 70 DEG C, grind
Obtain cabo biological carbon materials.Cabo charcoal will be obtained and use KOH activator aqueous solution (KOH
Mole percent is 5mol%) mix postactivated 2h, after drying with 1: 4 ratio (solid-liquid weight ratio)
Calcine 2h under nitrogen protection at 600 DEG C, clean to neutral with deionized water after natural cooling, be dried
After i.e. obtain charcoal.The charcoal SEM figure prepared is shown in Fig. 3.
The particle size of obtained charcoal is 0.8 μm, and specific surface area is 560m2/g。
Embodiment 4:
Tobacco stem waste after crushed, chooses the granule of 60 mesh, is 1g: 12ml according to solid-to-liquid ratio
After 5g cabo biomass and 60ml deionized water are stirred by ratio, it is encapsulated in autoclave
, under conditions of electric furnace heating rate is 10～20 DEG C/min, carry out hydro-thermal carbonization 5h in 180 DEG C,
Use deionized water wash to neutrality, sucking filtration after natural cooling, after being dried 10h at 70 DEG C, grind
Obtain cabo biological carbon materials.Cabo charcoal will be obtained and use KOH activator aqueous solution (KOH
Mole percent is 5mol%) mix postactivated 2h, after drying with 1: 4 ratio (solid-liquid weight ratio)
Calcine 2h under nitrogen protection at 800 DEG C, clean to neutral with deionized water after natural cooling, be dried
After i.e. obtain charcoal.The charcoal SEM figure prepared is shown in Fig. 4.
The particle size of obtained charcoal is 1.0 μm, and specific surface area is 540m2/g。
Embodiment 5:
Tobacco stem waste after crushed, chooses the granule of 60 mesh, is 1g: 12ml according to solid-to-liquid ratio
After 5g cabo biomass and 60ml deionized water are stirred by ratio, it is encapsulated in autoclave
, under conditions of electric furnace heating rate is 10～20 DEG C/min, carry out hydro-thermal carbonization 2h in 200 DEG C,
Use deionized water wash to neutrality, sucking filtration after natural cooling, after being dried 10h at 70 DEG C, grind
Obtain cabo biological carbon materials.Cabo charcoal will be obtained and use KOH activator aqueous solution (KOH
Mole percent is 5mol%) mix postactivated 5h, after drying with 1: 4 ratio (solid-liquid weight ratio)
Calcine 2h under nitrogen protection at 400 DEG C, clean to neutral with deionized water after natural cooling, be dried
After i.e. obtain charcoal.The charcoal SEM figure prepared is shown in Fig. 5.
The particle size of obtained charcoal is 1.2 μm, and specific surface area is 520m2/g。
Embodiment 6:
Tobacco stem waste after crushed, chooses the granule of 60 mesh, is 1g: 12ml according to solid-to-liquid ratio
After 5g cabo biomass and 60ml deionized water are stirred by ratio, it is encapsulated in autoclave
, under conditions of electric furnace heating rate is 10～20 DEG C/min, carry out hydro-thermal carbonization 2h in 200 DEG C,
Use deionized water wash to neutrality, sucking filtration after natural cooling, after being dried 10h at 70 DEG C, grind
Obtain cabo biological carbon materials.Cabo charcoal will be obtained and use K2CO3Activator aqueous solution (K2CO3
Mole percent is 5mol%) mix postactivated 2h, after drying with 1: 4 ratio (solid-liquid weight ratio)
Calcine 2h under nitrogen protection at 600 DEG C, clean to neutral with deionized water after natural cooling, be dried
After i.e. obtain charcoal.The charcoal SEM figure prepared is shown in Fig. 6.
The particle size of obtained charcoal is 1.5 μm, and specific surface area is 480m2/g。
Embodiment 7:
Tobacco stem waste after crushed, chooses the granule of 60 mesh, is 1g: 12ml according to solid-to-liquid ratio
After 5g cabo biomass and 60ml deionized water are stirred by ratio, it is encapsulated in autoclave
, under conditions of electric furnace heating rate is 10～20 DEG C/min, carry out hydro-thermal carbonization 5h in 200 DEG C,
Use deionized water wash to neutrality, sucking filtration after natural cooling, after being dried 10h at 70 DEG C, grind
Obtain cabo biological carbon materials.Cabo charcoal will be obtained and use KOH activator aqueous solution (KOH
Mole percent is 10mol%) mix postactivated 2h, after drying with 1: 4 ratio (solid-liquid weight ratio)
Calcine 2h under nitrogen protection at 400 DEG C, clean to neutral with deionized water after natural cooling, be dried
After i.e. obtain charcoal.The charcoal SEM figure prepared is shown in Fig. 7.
The particle size of obtained charcoal is 1.8 μm, and specific surface area is 450m2/g。
Embodiment 8:
Tobacco stem waste after crushed, chooses the granule of 60 mesh, is 1g: 12ml according to solid-to-liquid ratio
After 5g cabo biomass and 60ml deionized water are stirred by ratio, it is encapsulated in autoclave
, under conditions of electric furnace heating rate is 10～20 DEG C/min, carry out hydro-thermal carbonization 5h in 200 DEG C,
Use deionized water wash to neutrality, sucking filtration after natural cooling, after being dried 10h at 70 DEG C, grind
Obtain cabo biological carbon materials.Cabo charcoal will be obtained and use K2CO3Activator aqueous solution (K2CO3
Mole percent is 5mol%) mix postactivated 2h, after drying with 1: 4 ratio (solid-liquid weight ratio)
Calcine 2h under nitrogen protection at 400 DEG C, clean to neutral with deionized water after natural cooling, be dried
After i.e. obtain charcoal.The charcoal SEM figure prepared is shown in Fig. 8.
The particle size of obtained charcoal is 2.0 μm, and specific surface area is 420m2/g。
Comparative example 1
Tobacco stem waste after crushed, chooses the granule of 60 mesh, is 1g: 12ml according to solid-to-liquid ratio
After 5g cabo biomass and 60ml deionized water are stirred by ratio, it is encapsulated in autoclave,
Under conditions of electric furnace heating rate is 10～20 DEG C/min, carry out hydro-thermal carbonization 5h in 150 DEG C, from
So use deionized water wash to neutrality, sucking filtration after cooling, after being dried 10h at 70 DEG C, grind
To cabo biological carbon materials (unactivated).
The holes of products volume directly using hydro-thermal charring to prepare is the highest, and reaction carries out slowly, absorption effect
The most inconspicuous.Containing cellulose and lignin in cabo, and other small-molecule substance, simple water
Hot carbonization process after, it is thus achieved that material composition kind few.
The biological carbon material and the four kinds of concentration that each embodiment and comparative example are prepared are 10～1000ppm
Heavy metal ion solution is in the ratio mixing that solid-to-liquid ratio is 0.01g～0.50g: 5～50ml, and vibrate 24h,
Heavy metal ion solution concentration after utilizing atomic absorption spectrophotometer to measure absorption.
Each embodiment prepares the heavy metal ion adsorbed amount detection data of charcoal sample and is shown in Table
1 (mg/g is heavy metal mg of every g activated carbon adsorption.).
Table 1
As shown in Table 1, the charcoal prepared after the activation of each embodiment has good heavy metal adsorption effect.
Claims (10)
1. one kind utilizes the method that cabo prepares charcoal, it is characterised in that comprise the following steps:
Step (1): cabo carries out hydro-thermal carbonization reaction with water after pulverizing at 180 DEG C～260 DEG C；
Reaction sequentially pass through again after terminating filtrations, wash, dry；
Step (2): again at inert atmosphere after the activation of activated dose of step (1) dried product
Calcine at 400 DEG C～1200 DEG C, wash subsequently, be drying to obtain charcoal；Described activator is Louis
At least one in this acid, peroxide, alkali metal hydroxide, alkali carbonate.
Utilize the method that cabo prepares charcoal the most as claimed in claim 1, it is characterised in that cigarette
Granularity after stalk is pulverized is 40～100 mesh.
Utilize the method that cabo prepares charcoal the most as claimed in claim 2, it is characterised in that step
Suddenly, in (1), cabo is 1g: 2～15ml with the w/v of water.
Utilize the method that cabo prepares charcoal the most as claimed in claim 1, it is characterised in that water
During hot carbonization reaction, heating rate is 10～20 DEG C/min.
Utilize the method that cabo prepares charcoal the most as claimed in claim 1, it is characterised in that institute
The activator stated is ZnCl2、SnCl2、H3PO4、H2O2, KOH or K2CO3In at least one.
Utilize the method that cabo prepares charcoal the most as claimed in claim 5, it is characterised in that live
In the aqueous solution of agent, described activator mole percent is 1mol%～10mol%, activation process
In, the mass ratio of the cabo of step (1) and the aqueous solution of activator is 1: 1～5.
Utilize the method that cabo prepares charcoal the most as claimed in claim 6, it is characterised in that step
Suddenly, in (2), soak time is 1～10 hour.
Utilize the method that cabo prepares charcoal the most as claimed in claim 1, it is characterised in that forge
Burning process is carried out under nitrogen protection, and wherein, the flow velocity of nitrogen is 0.8～1.1L/min.
9. one kind uses the charcoal that method described in any one of claim 1～8 prepares.
10. the application of charcoal Adsorption of Heavy Metals described in a claim 9, it is characterised in that will
Described charcoal contacts with the sample solution containing heavy metal.
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