CN107684898A - A kind of method that trace oxygen atmosphere pyrolysis prepares mao bamboon charcoal - Google Patents
A kind of method that trace oxygen atmosphere pyrolysis prepares mao bamboon charcoal Download PDFInfo
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- CN107684898A CN107684898A CN201710734276.6A CN201710734276A CN107684898A CN 107684898 A CN107684898 A CN 107684898A CN 201710734276 A CN201710734276 A CN 201710734276A CN 107684898 A CN107684898 A CN 107684898A
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- mao bamboon
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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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- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
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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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- 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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- 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- Life Sciences & Earth Sciences (AREA)
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- Hydrology & Water Resources (AREA)
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- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The method for preparing mao bamboon charcoal is pyrolyzed the invention discloses a kind of trace oxygen atmosphere, is comprised the following steps:S1. mao bamboon is preprocessed, to fragmentation status that is clean and drying;S2. pretreated mao bamboon is pyrolyzed through trace oxygen atmosphere, the trace oxygen atmosphere is the mixed gas of oxygen and nitrogen, and in the mixed gas, the volume ratio of oxygen is 0% ~ 4%;S3. by thermal decomposition product in step S2, after pulverizing and sieving, mao bamboon charcoal is obtained.The method that trace oxygen atmosphere pyrolysis proposed by the present invention prepares mao bamboon charcoal, adsorbs heavy metal lead applied to removing in water body, efficiently solves the shortcomings of water environment heavy metals removal process adsorption capacity is low, cost is too high.
Description
Technical field
The present invention relates to biological carbon materials preparing technical field, it particularly relates to a kind of trace oxygen atmosphere pyrolysis system
The method of standby mao bamboon charcoal.
Background technology
Heavy metal is mostly non-degradable type noxious material, does not possess natural purifying ability, once it is difficult into environment from ring
Removed in border.The administering method of heavy metal pollution at present is based on physico-chemical process, and bioremediation technology is as economical, high
Effect, the Treatment process of environmental protection also receive significant attention.Using super enriching plant from water body by landfill to plant top,
Artificial harvest transfer, it is used to extract heavy metal after burning, it is turned waste into wealth.Therefore bioremediation technology feasibility and effectively
Property will gradually strengthen, administer and prevent and treat heavy metal pollution in terms of will play a greater role, have a good application prospect.
The administering method of heavy metal pollution of water body generally speaking, using following two Basic Ways, first, reducing heavy metal
Transfer ability and bioavailability in water body;Second, heavy metal is thoroughly removed from contaminated water body.Specifically carry out book,
There are as below methods for tool:
1. coagulant sedimentation, adding alkaline matter, raising water pH value, most of heavy metal generation hydroxide can be made to sink
Form sediment.
2. ion reduction method and exchange process, the heavy metal in water body is reduced using the reducing agent that some are readily obtained, shape
Into pollution-free or lighter pollution level compound, so as to reduce migration and bioavailability of the heavy metal in water body,
To mitigate pollution of the heavy metal to water body.
3. technology of Electrodynamics Renovation, DC electric field is added to the water body both ends by heavy metal pollution, is migrated using electric field
Power is by heavy metal transformation water-outlet body.
4. phytoremediation, the technology for being implemented pollution environmental improvement using specified plant is referred to as, and passes through plant heavy metal
Element or the special enrichment of organic substance and degradation capability are made a return journey except the pollutant in environment, or eliminate the toxicity of pollutant, are reached
The huge sum of money such as Cd, Cr and Cu in sewage can be removed well to the purpose of pollution control and restoration of the ecosystem, such as Eichhornia crassipes, Chinese celery
Category.
5. animal reparation method, absorb, be enriched with water body using some preferable fish and other aquatic animal species
Heavy metal, then they are displaced from water body, to reach the purpose of heavy metal pollution of water body reparation.
6. microorganism remediation method, the conversion of main fixation and form including microorganism heavy metal.
The shortcomings that cost is too high be present in above method, although and above method 4 ~ 6 comparatively cost is relatively low, deposit
It is poor in instantaneity, the shortcomings that adsorption capacity is low, how to solve water environment heavy metals removal process adsorption capacity is low, cost it is too high this
One technical problem is the technical problem that solution is paid close attention in this area all the time.
The problem of in correlation technique, effective solution is not yet proposed at present.
The content of the invention
For the above-mentioned technical problem in correlation technique, the present invention proposes that a kind of trace oxygen atmosphere pyrolysis prepares mao bamboon life
The method of thing charcoal, heavy metal lead is adsorbed applied to removing in water body, efficiently solve the absorption of water environment heavy metals removal process and hold
Measure the shortcomings of low, cost is too high.
To realize above-mentioned technical purpose, the technical proposal of the invention is realized in this way:
A kind of method that trace oxygen atmosphere pyrolysis prepares mao bamboon charcoal, comprises the following steps:
S1. mao bamboon is preprocessed, to fragmentation status that is clean and drying;
S2. pretreated mao bamboon is pyrolyzed through trace oxygen atmosphere, the trace oxygen atmosphere is the mixing of oxygen and nitrogen
Gas, in the mixed gas, the volume ratio of oxygen is 0% ~ 4%;
S3. by thermal decomposition product in step S2, after pulverizing and sieving, mao bamboon charcoal is obtained.
Further, the pretreatment specifically comprises the following steps:By fresh adult mao bamboon place dry place air-dry, with surpass
Pure water rinsing 3 times, baking 24h in 105 DEG C of baking ovens is positioned over, is cleaned, dried with ultra-pure water after crushing.Carry out according to the method described above
Pretreatment, can remove the influence of dust and moisture to pyrolytic process, make the charcoal purity that finally gives higher, heavy metal
The absorption property of ion is more preferable, cleaning and drying after especially crushing, can allow shadow except dust and moisture to pyrolytic process
Sound minimizes.
Further, the breaking method is that mao bamboon is cut into 1cm × 1cm fragment by chopper, is sieved through with nylon wire
Sieve, obtains the mao bamboon fragment of 80 ~ 100 mesh.
Further, the breaking method is directly to use mao bamboon and cut into fragment of the length for 5 ~ 10cm.
Further, step S2 specifically comprises the following steps:
Pretreated mao bamboon is put into vacuum tube furnace by step A., uses O2And N2Sky in mixed gas displacement vacuum tube furnace
Gas;
Step B. is pyrolyzed to the mao bamboon in vacuum tube furnace, and pyrolytic process is continually fed into O2And N2Mixed gas is until reaction
Terminate.
Further, O is used in the step A2And N2The method of air in mixed gas displacement vacuum tube furnace is specific
For:To electron tubes type stove evacuation, reach -0.1Mpa to vacuum, be passed through O2And N2Mixed gas, recover normal pressure, repeat above-mentioned
Operation is once.By this mode displaced air, the air pocket in vacuum tube furnace can be made to be reduced to pyrolytic process almost
The degree that can not be impacted.
Further, the method being pyrolyzed in the step B to the mao bamboon in vacuum tube furnace is specially:Open vacuum
The air outlet valve of tube furnace, the flow of outlet is maintained 200 ml/min, be warming up to 450 DEG C with 20 DEG C/min speed, keep 1
~ 8 hours, preferably 2 ~ 4 hours, it can both ensure that pyrolysis is complete, the waste of multiple-energy-source and material will not be produced again;It was pyrolyzed
Journey is continually fed into O2And N2Mixed gas, terminate until reacting, tube furnace is down to room temperature.
Further, the mao bamboon can be replaced with firm bamboo.
Further, the vacuum tube furnace can be replaced with atmosphere Muffle furnace.
Beneficial effects of the present invention:(1)Rapid using growth, Economic Bamboo mao bamboon is easy to get as raw material, material, beneficial to life
The large-scale production of thing charcoal, manufacture craft is succinct, low production cost.
(2)Using trace oxygen copyrolysis, the addition of oxygen, contribute to the increasing of charcoal ash composition type and quantity
Add, improve heavy metal adsorption effect.
(3)The present invention prepares gained sorbing material and effectively lifts heavy metal lead adsorption capacity, and Heavy Metals in Water Environment is inhaled
Attached capacity reaches 35.4 mgg;With higher economy and application value.
Brief description of the drawings
Fig. 1 is the surface sweeping electron microscope of the mao bamboon charcoal prepared in present example four;
Fig. 2 is the surface sweeping electron microscope after the mao bamboon charcoal adsorpting lead ion prepared in present example four;
Fig. 3 is the infrared spectrogram of the mao bamboon charcoal prepared in present example four;
Fig. 4 is X-ray diffractogram after the biological adsorpting lead ion of the mao bamboon prepared in present example four;
Fig. 5 is adsorption effect comparison chart of the different pyrolysis oxygen content mao bamboon charcoals to Lead in Aqueous Solution.
Embodiment
Below in conjunction with specific embodiment, technical scheme is clearly and completely described, embodiment is only used
In explaining the present invention, not limiting the present invention.
Embodiment one
Fresh adult mao bamboon places that to dry place air-dried, with ultrapure water 3 times, removes skim-coat dust, is positioned in 105 DEG C of baking ovens
24h is toasted, 1cm × 1cm fragment is cut into by chopper, nylon wire is sieved through sieve, obtains the mao bamboon fragment of 80 ~ 100 mesh, use is ultrapure
After water is washed 3 times, 90 DEG C of ± 2 DEG C of drying 5h are placed in.
Pretreated mao bamboon is put into vacuum tube furnace, vacuumized, reaches -0.1Mpa to vacuum, then passes to O2
And N2Mixed gas, in the mixed gas, O2Volume ratio is 0%, recover normal pressure after, repetition vacuumize, aeration once,
Recover normal pressure again.
The air outlet valve of vacuum tube furnace is opened, the flow of outlet is maintained 200 ml/min, with 20 DEG C/min speed
450 DEG C are warming up to, keeping temperature 4 hours, pyrolytic process is continually fed into O2And N2Mixed gas, until reaction terminates tube furnace drop
To room temperature.
After thermal decomposition product is pulverized and sieved, charcoal is obtained.
Embodiment two
The difference of embodiment two and embodiment one is, in the mixed gas, O2Volume ratio is 1%.
Embodiment three
The difference of embodiment three and embodiment one is, in the mixed gas, O2Volume ratio is 2%.
Example IV
The difference of example IV and embodiment one is, in the mixed gas, O2Volume ratio is 4%.
Embodiment five
The difference of embodiment five and example IV is, mao bamboon is replaced with to firm bamboo in belonging to together.
Embodiment six
The difference of embodiment six and example IV is, vacuum tube furnace is replaced with into atmosphere Muffle furnace.
Embodiment seven
The difference of embodiment seven and example IV is, breaking method be mao bamboon is directly used cut into length for 5 ~
10cm fragment.
Charcoal obtained by above-described embodiment one to embodiment seven is subjected to testing adsorption effect, assay method includes such as
Lower step:It is 0.08g to configure the leaded ml of 100 mg/L nitric acid cadmium solution 40 and P1 mass is added in centrifuge tube, and setting 3 is parallel
Sample, set and do not add the dummy of charcoal, centrifuge tube is then positioned in 150r/min constant incubators into 24 DEG C shakes
24h is swung, supernatant is taken after centrifugation, remaining lead ion content in equilibrium liquid is determined using ICP-OES, so as to obtain charcoal absorption
Amount.Analysis result is as follows:
Embodiment one to four is compared and understood, works as O2When volume ratio is 4%, the charcoal ash content of obtained charcoal contains
Highest is measured, to lead ion adsorbance also highest.
Example IV is understood compared with embodiment five, mao bamboon is replaced with into firm bamboo, obtains the heavy ion of charcoal
Adsorption effect is also very good.
Example IV is understood compared with embodiment six, is pyrolyzed using atmosphere Muffle furnace, obtains charcoal
Heavy ion adsorption effect is also very good.
Example IV is understood compared with embodiment seven, is crushed by the way of direct shearing, obtains biology
The heavy ion adsorption effect of charcoal is also very good.
The adsorbance that gained charcoal in example IV is carried out to heavy metal containing sewage is tested, and is measured adsorption capacity and is reached 35.4
mg/g。
The present invention is by using mao bamboon as raw material, in trace oxygen(1%-4% oxygen contents)Under atmosphere, high temperature pyrolysis generation is rich
Carbon containing charcoal.The cost of raw material is relatively low, and obtained charcoal has larger specific surface area and porosity, heavy metal lead
Ion has the adsorption effect of broad spectrum activity, and non-secondary pollution.With pyrolysis oxygen content increase, charcoal under the conditions of 450 DEG C
The adsorption capacity of heavy metal lead dramatically increases.It is an advantage of the invention that:By introducing trace oxygen, prepare charcoal ash content and show
Increase is write, so as under the conditions of low temperature pyrogenation, obtain efficient heavy metal absorbent.
In summary, the charcoal prepared as raw material using mao bamboon, can be applied to remove heavy metal lead ion in water environment
Process.The problem of adsorption effect is poor, cost is high in the existing adsorption technology heavy metal adsorption process of customer service of the present invention;Biology simultaneously
The carbonisation of charcoal, causes carbonic acid to seal up for safekeeping in charcoal, reduces greenhouse gases CO2Discharge, it is beneficial to environmental ecology effects.
Claims (9)
1. a kind of method that trace oxygen atmosphere pyrolysis prepares mao bamboon charcoal, it is characterised in that comprise the following steps:
S1. mao bamboon is preprocessed, to fragmentation status that is clean and drying;
S2. pretreated mao bamboon is pyrolyzed through trace oxygen atmosphere, the trace oxygen atmosphere is the mixing of oxygen and nitrogen
Gas, in the mixed gas, the volume ratio of oxygen is 0% ~ 4%;
S3. by thermal decomposition product in step S2, after pulverizing and sieving, mao bamboon charcoal is obtained.
2. the method that a kind of trace oxygen atmosphere pyrolysis according to claim 1 prepares mao bamboon charcoal, it is characterised in that
The pretreatment specifically comprises the following steps:Fresh adult mao bamboon is placed into the place of drying to air-dry, with ultrapure water 3 times, placement
In toasting 24h in 105 DEG C of baking ovens, cleaned, dried with ultra-pure water after crushing.
3. the method that a kind of trace oxygen atmosphere pyrolysis according to claim 2 prepares mao bamboon charcoal, it is characterised in that
The breaking method is that mao bamboon is cut into 1cm × 1cm fragment by chopper, is sieved through sieve with nylon wire, obtains 80 ~ 100 purposes
Mao bamboon fragment.
4. the method that a kind of trace oxygen atmosphere pyrolysis according to claim 2 prepares mao bamboon charcoal, it is characterised in that
The breaking method is directly to use mao bamboon and cut into fragment of the length for 5 ~ 10cm.
5. the method that a kind of trace oxygen atmosphere pyrolysis according to claim 1 prepares mao bamboon charcoal, it is characterised in that
Step S2 specifically comprises the following steps:
Pretreated mao bamboon is put into vacuum tube furnace by step A., uses O2And N2Sky in mixed gas displacement vacuum tube furnace
Gas;
Step B. is pyrolyzed to the mao bamboon in vacuum tube furnace, and pyrolytic process is continually fed into O2And N2Mixed gas is until reaction
Terminate.
6. the method that a kind of trace oxygen atmosphere pyrolysis according to claim 5 prepares mao bamboon charcoal, it is characterised in that
O is used in the step A2And N2The method of air in mixed gas displacement vacuum tube furnace is specially:Vacuum tube furnace is taken out very
Sky, reach -0.1Mpa to vacuum, be passed through O2And N2Mixed gas, recover normal pressure, repeat aforesaid operations once.
7. the method that a kind of trace oxygen atmosphere pyrolysis according to claim 5 prepares mao bamboon charcoal, it is characterised in that
The method being pyrolyzed in the step B to the mao bamboon in vacuum tube furnace is specially:The air outlet valve of vacuum tube furnace is opened, is made
The flow of outlet is maintained 200 ml/min, is warming up to 450 DEG C with 20 DEG C/min speed, is kept for 1 ~ 8 hour, pyrolytic process is held
It is continuous to be passed through O2And N2Mixed gas, terminate until reacting, tube furnace is down to room temperature.
8. the method that a kind of trace oxygen atmosphere pyrolysis according to claim 5 prepares mao bamboon charcoal, it is characterised in that
The mao bamboon can be replaced with firm bamboo.
9. the method that a kind of trace oxygen atmosphere pyrolysis according to claim 5 ~ 7 prepares mao bamboon charcoal, its feature exist
In the vacuum tube furnace can be replaced with atmosphere Muffle furnace.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110624504A (en) * | 2019-09-30 | 2019-12-31 | 河北大学 | Method for preparing biochar by carbonizing biological straw through low-temperature oxygen control |
CN111423280A (en) * | 2019-01-08 | 2020-07-17 | 湖南农业大学 | 3D-structure biochar fertilizer and preparation method and application thereof |
CN114314816A (en) * | 2022-01-10 | 2022-04-12 | 湖南云河信息科技有限公司 | Method for removing heavy metal chromium by mixed biological calcination |
CN114538408A (en) * | 2020-11-24 | 2022-05-27 | 中国科学院广州能源研究所 | Method for preparing high electrocatalytic activity biochar through micro-aerobic pyrolysis |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111423280A (en) * | 2019-01-08 | 2020-07-17 | 湖南农业大学 | 3D-structure biochar fertilizer and preparation method and application thereof |
CN110624504A (en) * | 2019-09-30 | 2019-12-31 | 河北大学 | Method for preparing biochar by carbonizing biological straw through low-temperature oxygen control |
CN114538408A (en) * | 2020-11-24 | 2022-05-27 | 中国科学院广州能源研究所 | Method for preparing high electrocatalytic activity biochar through micro-aerobic pyrolysis |
CN114314816A (en) * | 2022-01-10 | 2022-04-12 | 湖南云河信息科技有限公司 | Method for removing heavy metal chromium by mixed biological calcination |
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