CN104549154B - The preparation method of the charcoal of cadmium in the safe adsorbed water body of energy - Google Patents
The preparation method of the charcoal of cadmium in the safe adsorbed water body of energy Download PDFInfo
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- CN104549154B CN104549154B CN201510033721.7A CN201510033721A CN104549154B CN 104549154 B CN104549154 B CN 104549154B CN 201510033721 A CN201510033721 A CN 201510033721A CN 104549154 B CN104549154 B CN 104549154B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/485—Plants or land vegetals, e.g. cereals, wheat, corn, rice, sphagnum, peat moss
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/40—Capture or disposal of greenhouse gases of CO2
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- Water Supply & Treatment (AREA)
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- Carbon And Carbon Compounds (AREA)
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Abstract
The invention discloses the preparation method of the biomass carbon of cadmium in a kind of safe adsorbed water body of energy, comprise the following steps：1), will be air-dried after harvested napier grass removal of impurities, then crushed successively, dried；2), crush the napier grass after drying to be put into retort, being then warming up to 480~520 DEG C with the speed of 4~6 DEG C/min carries out oxygen barrier carbonization reaction, 1.8~2.2h of insulation reaction；3), by step 2) obtained by charing after napier grass be cooled to room temperature, pulverize and sieve, obtain biomass carbon.Instant invention overcomes adsorption efficiency is not high, be easily caused secondary pollution and relatively costly this three major issues during existing adsorption technology improvement heavy metal containing sewage；Stabilization has been carried out to carbon in plant refuse simultaneously to seal up for safekeeping, CO2 emission has been reduced, with significant ecological benefits.
Description
Technical field
The present invention relates to a kind of preparation of biological carbon materials, belong to technical field of biomass resource utilization.It is more particularly to a kind of
The biological carbon materials and preparation method of cadmium in the safe adsorbed water body of energy.
Background technology
With developing rapidly for current industrial and agricultural production, heavy metal passes through mining, metal smelt, chemical production wastewater
And agriculture chemical use and the number of ways such as house refuse enter water body, cause the heavy metal in water being on the rise dirty
Dye.Additionally, the features such as heavy metal pollution also has disguised, chronicity and irreversibility, and human body can be entered by food chain
So as to endanger the life and health of the mankind, this causes that heavy metal pollution of water body turns into social concern urgently to be resolved hurrily.Wherein, cadmium pollution
Paid high attention to by people from after Japanese " Itai-itai diseases " event.At present, the administration way of Heavy Metals in Waters pollution mainly has
Chemical precipitation method, ion-exchange resin, hyperfiltration, membrane separation process and absorption method etc..Wherein absorption method is efficient, cheap because of its
The advantages of with easily operated and small environmental perturbation, is used widely.
Charcoal be by biomass under anoxic conditions by high temperature pyrolysis produce a kind of stabilization height aromatization and
Solid matter rich in carbon, because having well-developed pore structure and larger specific surface area, preparing raw material is originated in addition
It is extensive and with low cost, become a kind of novel absorption material and received significant attention in environmental area.
At present, the heavy metal absorbent for being used in water process is mainly acticarbon and organically-modified material.And work as
Activated carbon of the present as adsorbent is to obtain use chemical activation method specific surface area higher more, and is needed after activation anti-with acid
Multiple cleaning, not only technique is cumbersome, relatively costly but also certain secondary pollution can be caused to environment.CN 103949214A are announced
A kind of heavy metal adsorption method for preparation of active carbon with Chinese medicine slag as raw material, adsorbent prepared by the method be by Chinese medicine slag by
Through high temperature carbonization and steam activation after the classification of rhizome mass of residue percentage composition, remixing rear and hydrogen peroxide aoxidize instead
Should, then it is modified through methacrylic acid and using crosslinking agent solidification, finally drying, crushing are prepared.Technique is more numerous
It is trivial, and preparation process consumes a large amount of organic reagents, considerably increases production cost, and have certain harm to environment.CN
104150480A discloses a kind of preparation method of Adsorption of Heavy Metals activated carbon with high specific surface area, and the method is former by biomass
Material dry, be crushed to 60~100 mesh after be put into microwave reactor, be passed through N2, it is 1000W~2000W, carbon to control microwave power
Changing 300~500 DEG C of temperature carries out microwave carbonization；After microwave carbonization, it is cooled to room temperature and obtains carbonized material, takes carbonized material and organic alkoxide
Activator presses 1:After 1~10 quality is more uniform than ground and mixed, it is put into atmosphere furnace and is warming up to the speed of 5~50 DEG C/min
800~1000 DEG C and be incubated 100~300min, be cooled to room temperature taking-up, through salt pickling after, then be washed to neutrality, dry, obtain final product
Activated carbon.The preparation method is equally complex process, and cost is high, is unsuitable for spread.Additionally, the activity of chemical modification
Although charcoal can apply to Industrial Waste Water Treatments heavy metal, the drinking water of Drinking w ater, reservoir upstream etc. can not be applied to
The absorption of heavy metal, easily causes secondary pollution.
Therefore, how to prepare a kind of environmentally friendly, efficient and with low cost heavy metal and there is good adsorption to Cadmium In The Water Body
The adsorbent of performance is particularly important.
The content of the invention
The technical problem to be solved in the present invention is to provide the preparation method of the charcoal of cadmium in a kind of safe adsorbed water body of energy.
Instant invention overcomes adsorption efficiency is not high, be easily caused secondary pollution and cost during existing adsorption technology improvement heavy metal containing sewage
This three major issues higher.
In order to solve the above-mentioned technical problem, the present invention provides a kind of preparation of the biomass carbon of cadmium in safe adsorbed water body of energy
Method, comprises the following steps：
1), will be air-dried after harvested napier grass removal of impurities, then crushed successively, dried；
2), crush the napier grass after drying to be put into retort, then with the speed of 4~6 DEG C/min (preferably 5 DEG C/min)
Being warming up to 480~520 DEG C (preferably 500 DEG C) carries out oxygen barrier carbonization reaction, 1.8~2.2h of insulation reaction (preferably 2h)；
3), by step 2) obtained by charing after napier grass be cooled to room temperature, pulverize and sieve, obtaining biomass carbon (can adsorb safely
The biomass carbon of Cadmium In The Water Body).
As the improvement of the preparation method of biomass carbon of the invention：
Step 2) in, be passed through during oxygen barrier carbonization reaction nitrogen make the pressure in charing furnace chamber maintain 0.04~
0.06MPa (preferably 0.05Mpa).
As the further improvement of the preparation method of biomass carbon of the invention：
Step 1) in,
Napier grass water content after air-drying is 10%~20% (quality %)；
It is crushed to particle diameter≤10mm；
2.5~3h is dried in 90~105 DEG C.
As the further improvement of the preparation method of biomass carbon of the invention：
The step 3) in the aperture that pulverizes and sieves be 60~100 mesh.
The purposes of the biomass carbon that the present invention is also prepared there is provided the above method simultaneously：As Heavy Metals in Waters cadmium
Adsorbent.
Remarks explanation：
Step 1) air-dry time be about one week.
Step 2) in, retort for example can select moveable box resistance atmosphere protection stove.
Napier grass (Pennisetum purpureum Schum), alias：Napier-grass, grass family, broomcorn millet race is perennial grows thickly
Large-scale herbaceous plant.Africa is originated in, nature and artificial swamp are grown on extensively as a kind of water remediation plant after introducing China
In.Harvested napier grass typically makees waste treatment, does not have practical value.
The present invention is relative to above-mentioned prior art technical advantage specific as follows：
1st, documents use microwave charring, and the requirement to equipment is high；And the present invention is set by the present invention
Under fixed process conditions, conventional retort is only needed；
2nd, documents complex operation step and consume mass energy and increased cost but the removal of heavy metal effect
Rate can not possibly have very big lifting, and can not be used for the heavy metal adsorption of drinking water source due to the addition of organic alkoxide；And this
Invention can guarantee that cadmium in highly effective and safe adsorbed water body under the process conditions set by the present invention, both, turn avoid organic alkoxide
Use.
Relative to the technology of preparing of existing adsorbent for heavy metal, the beneficial effects of the present invention are：
(1) present invention solves the problems, such as body eutrophication rehabilitation plant offal treatment, turns waste into wealth, by discarded object
Being made charcoal is carried out further with effectively prevent secondary pollution.
(2) present invention not only solves the problem there may be secondary pollution, Er Qiecai in conventional active carbon purifying water body
Material is easy to get, and manufacture craft is succinct, low production cost.
(3) heavy metal absorbent that the present invention is prepared is big to Heavy Metals in Waters adsorbance, and removal efficiency is very high；Its
To removal efficiency of heavy metals in drinking water source small watershed more than 97%；Therefore there is social and economic benefit higher.
In sum, the biomass carbon that the present invention is prepared using napier grass discarded object, can directly apply to water body purification
During removal cadmium.Administer during heavy metal containing sewage that adsorption efficiency is not high, easily lead instant invention overcomes existing adsorption technology
Cause secondary pollution and relatively costly this three major issues；Stabilization has been carried out to carbon in plant refuse simultaneously to seal up for safekeeping, has reduced two
Oxidation carbon emission, with significant ecological benefits.
Brief description of the drawings
Specific embodiment of the invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 is the electron-microscope scanning figure of napier grass charcoal (biomass carbon) prepared by the present invention.
Fig. 2 is the electron-microscope scanning figure after napier grass charcoal absorption cadmium prepared by the present invention.
Fig. 3 is the infrared spectrogram before and after napier grass charcoal absorption cadmium prepared by the present invention.
Fig. 4 is the energy spectrum diagram of napier grass charcoal prepared by the present invention.
Fig. 5 is the energy spectrum diagram after napier grass charcoal absorption cadmium prepared by the present invention.
Fig. 6 is that the present invention utilizes charcoal prepared by napier grass and other water remediation plants to water body cadmium adsorption efficiency ratio
Compared with.
Remarks explanation：It is that nitric acid cadmium solution as described in experiment 3 is 100mg/L that " absorption cadmium after " is corresponding in above-mentioned figure
When.
Specific embodiment
The present invention is described in further detail with reference to embodiment, but it is necessary to note that following embodiment is only used
In the explanation present invention, but it is not construed as limiting the invention.
The preparation method of embodiment 1, biomass carbon, follows the steps below successively：
Harvested napier grass is placed under ventilated environment after natural air drying one week (now, moisture content is 12%) chopping, mill
Into the powder of particle diameter≤10mm, place into baking oven and dry 3h in 105 DEG C；Be then placed in retort, be passed through nitrogen, and with 5 DEG C/
The speed of min is warming up to 500 DEG C and carries out oxygen barrier carbonization reaction, and nitrogen is passed through during oxygen barrier carbonization reaction makes charing furnace chamber
Interior pressure maintains 0.05Mpa；Insulation reaction 2h；Then room temperature is cooled to, granular gains was crushed into 60-100
Mesh sieve, obtains powdered biomass carbon (hereinafter referred to as biomass charcoal powder).
Biomass charcoal powder (BC500) yield that the present embodiment is obtained is 38.72%, and its specific surface area is 43.36m2/ g, hole
It is 0.0241cc/g to hold, and aperture is 1.688nm, and micropore development is complete, and porosity is preferable；Its pH is 10.1, can be used as acid soil
Earth modifying agent；Its content of ashes is 35.25%, and cation exchange capacity (CEC) is 39.21cmol/kg, and K contents are 77.86mg/kg, can
As soil additive, and the content of beary metal such as Cd, Pb does not almost have, will not to water body produce pollution, to environmental hazard compared with
It is small, the absorption of heavy metal in polluted water body can be further used for.
Adsorption effect is by taking the following experiment of cadmium in charcoal product adsorbed water body as an example.
Experiment 1,
Charcoal sample (BC500) obtained by above-described embodiment 1 is carried out into adsorption test, is comprised the following steps：Weigh life
Thing charcoal sample (BC500) 0.05g adds the nitric acid cadmium solution 50mL containing cadmium 20mg/L in 100mL conical flasks, sets three weights
It is multiple, taper bottle closure is then placed in 25 DEG C of vibration 24h on the constant-temperature table of 160r/min, most pipette supernatant through membrane filtration afterwards
Liquid, using remaining cadmium concentration in ICP-MS measure equilibrium liquids, calculating is analyzed to its adsorbance.Through analysis, the flat of cadmium is obtained
Weighing apparatus concentration and adsorbance, biological carbon adsorbent are 19.2mg/g to the maximal absorptive capacity of cadmium, and removal efficiency is 98%.
Experiment 2, the concentration of the nitric acid cadmium solution that will be tested in 1 make 50mg/L into by 20mg/L, and remaining is equal to experiment 1.
Biological carbon adsorbent is 49.2mg/g to the maximal absorptive capacity of cadmium, and removal efficiency is 98.4%.
Experiment 3, the concentration of the nitric acid cadmium solution that will be tested in 1 make 100mg/L into by 20mg/L, and remaining is equal to experiment 1.
Biological carbon adsorbent is 97.4mg/g to the maximal absorptive capacity of cadmium, and removal efficiency is 97.4%.
Comparative example 1,
After harvested napier grass is placed under ventilated environment into natural air drying one week, then as described in CN 104150480A
Proceed as follows：
It is put into microwave reactor after being crushed to 60~100 mesh, is passed through N2(pressure in microwave reactor is controlled to be
0.05MPa), control microwave power carries out microwave carbonization for 2000W, 500 DEG C of carburizing temperature, and the time is 2 hours；Microwave is carbonized
Afterwards, room temperature is cooled to, carbonized material is obtained.
Comparative example 2, " biomass charcoal powder " of the gained of embodiment 1 is lived as described in CN 104150480A with organic alkoxide
Agent presses 1:After 5 quality is more uniform than ground and mixed, to be put into atmosphere furnace and be warming up to 1000 DEG C with the speed of 25 DEG C/min and protect
Warm 300min, is cooled to room temperature taking-up, through salt pickling after, then be washed to neutrality, dry, obtain final product activated carbon.
Comparative example 3, by embodiment 1 " air-dry after wear into particle diameter less than 10mm powder " make into " and air-dry after directly mill
Into 60-100 mesh sieves can be crossed ", and cancel " granular gains were crushed into 60-100 mesh sieves " at end accordingly；Remaining
Content is equal to embodiment 1.
Comparative example 4, will be raw materials used in above-described embodiment 1 -- napier grass changes mullet grass, thaliadeabata, cyperus alternifolius, water into respectively
Green onion, green reed, vetiver and water hyacinth this seven kinds of plants, remaining content is equal to embodiment 1.
Above-mentioned comparative example 1-4 gains are examined according to above-mentioned experiment 3 (cadmium initial concentration is 100mg/L) methods described
Survey, acquired results are as shown in table 1 and Fig. 6.
Table 1
| Maximal absorptive capacity (mg/g) | Removal efficiency | |
| Comparative example 1 | 83.8 | 83.8% |
| Comparative example 2 | 91.7 | 91.7% |
| Comparative example 3 | 94.4 | 94.4% |
Finally, in addition it is also necessary to it is noted that listed above is only several specific embodiments of the invention.Obviously, this hair
It is bright to be not limited to above example, there can also be many deformations.One of ordinary skill in the art can be from present disclosure
The all deformations directly derived or associate, are considered as protection scope of the present invention.
Claims (2)
1. can in safe adsorbed water body the biomass carbon of cadmium preparation method, it is characterized in that comprising the following steps：
1), will be air-dried after harvested napier grass removal of impurities, then crushed successively, dried；
Napier grass water content after air-drying is 10%~20%, is crushed to particle diameter≤10mm, and 2.5~3h is dried in 90~105 DEG C；
2), crush the napier grass after drying to be put into retort, being then warming up to 480~520 DEG C with the speed of 4~6 DEG C/min enters
Row oxygen barrier carbonization reaction, 1.8~2.2h of insulation reaction；
Nitrogen is passed through during oxygen barrier carbonization reaction makes the pressure in charing furnace chamber maintain 0.04~0.06Mpa；
3), by step 2) obtained by charing after napier grass be cooled to room temperature, crushed the sieve of 60~100 mesh, obtain biomass carbon.
2. the purposes of the biomass carbon that method as claimed in claim 1 is prepared, it is characterized in that：As Heavy Metals in Waters cadmium
Adsorbent.
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| CN104923153A (en) * | 2015-05-07 | 2015-09-23 | 浙江大学 | Preparation method for Canna biological carbon capable of simultaneously adsorbing ammonia nitrogen and cadmium |
| CN105126754A (en) * | 2015-09-02 | 2015-12-09 | 上海大学 | Method for removing chromium in water through biochar through corn straw |
| CN106693895B (en) * | 2017-01-17 | 2019-03-22 | 上海理工大学 | A kind of technique using low-quality charcoal processing lignite upgrading waste water |
| CN106902738A (en) * | 2017-03-10 | 2017-06-30 | 扬州大学 | A kind of wooden sub- shell base ecological restoration material and its application |
| CN107081129A (en) * | 2017-04-28 | 2017-08-22 | 广州大学 | A kind of charcoal and preparation method and application |
| CN107321305A (en) * | 2017-06-29 | 2017-11-07 | 湖南农业大学 | The preparation method of southern reed base modification biological charcoal and southern reed base modification biological charcoal and application |
| CN107721748B (en) * | 2017-11-14 | 2021-05-14 | 湖南农业大学 | Fixation of CO in air by using carbon sink grass2Method, carbon-sink grass carbon-based cadmium-reducing soil conditioner and preparation method and application thereof |
| CN108686622A (en) * | 2018-08-24 | 2018-10-23 | 合肥德博生物能源科技有限公司 | The preparation facilities and preparation method of a kind of modified biomass charcoal for soil remediation |
| CN113070026B (en) * | 2021-03-04 | 2022-07-01 | 浙江工业大学 | Preparation method and application of KOH-modified sedum alfredii hydrothermal carbon |
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