CN109621897A - The preparation method and its device and purposes of a kind of magnetic bio Carbon Materials - Google Patents
The preparation method and its device and purposes of a kind of magnetic bio Carbon Materials Download PDFInfo
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- CN109621897A CN109621897A CN201910004100.4A CN201910004100A CN109621897A CN 109621897 A CN109621897 A CN 109621897A CN 201910004100 A CN201910004100 A CN 201910004100A CN 109621897 A CN109621897 A CN 109621897A
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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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
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/343—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the pharmaceutical industry, e.g. containing antibiotics
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- Hydrology & Water Resources (AREA)
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- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Treatment Of Sludge (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The present invention relates to a kind of preparation method of magnetic bio Carbon Materials and its device and purposes; include the following steps: that sludge of sewage treatment plant is carried out to high temperature anaerobic pyrolysis obtains sludge organism charcoal; then it carries out dry method fine grinding and obtains charcoal powder; dry type magnetic separation is carried out to sludge organism carbon powder, obtains magnetic material, the particulate material obtained after conditioned and granulation; high temperature sintering is carried out under protective atmosphere; sintered material is obtained, furnace cooling obtains the magnetic bio Carbon Materials of porous structure.The present invention isolates a kind of magnetic material from pyrolyzing sludge product charcoal, and it is used to prepare magnetic bio Carbon Materials and is removed for fluoroquinolone antibiotics such as Ciprofloxacin efficient absorption, realize the resource utilization of sludge organism charcoal, reduce the preparation cost of adsorbent material, simple process, application is strong, with good economic efficiency and environmental benefit.
Description
Technical field
Utilization and antibiotic waste water processing technology field the present invention relates to sludge organism charcoal, especially a kind of magnetic green
The preparation method and its device and purposes of object Carbon Materials.
Background technique
Fluoroquinolones (fluoroquinolones, FQs) antibiotic is introduced on the basis of quinolone antibiotics
What fluorine atom was developed, be a kind of fully synthetic broad spectrum antibiotic.FQs treat as people and animal because of bacterium infection caused by disease
In disease, significant effect has good pharmacokinetic properties, has obtained widely answering in pharmaceuticals industry and animal husbandry
With.2009, usage amount had been located in anti-infectives forefront, occupied the 17% of the global antibiotic market share.Studies have shown that
The metabolic rate of FQs in vivo is less than 25%, and in vivo except small part residual, 75% or more is passed through in the form of raw medicine and metabolite
It is excreted by the fecaluria of patient and animal.It, can be by adsorbing, moving since its chemical property is more stable after FQs enters environment
It moves and a series of processes such as biological concentration is present in each surrounding medium, be particularly present in environment water, to endanger ring
Different kind organism in border induces and propagates all kinds of antibiotic resistant bacterias, destroys ecological environment.Literature survey is it is found that in environment
Various water bodys in (sewage treatment plant, hospital wastewater, breeding wastewater, surface water, underground water, drinking water etc.) have the inspection of FQs
Out.Wherein higher with the concentrations of Ciprofloxacin, Norfloxacin, Ofloxacin, pollution is more universal, in surface water, underground
(" removal of the During High-Temperature Composting to fluoroquinolone antibiotics in chicken manure ", Meng Lei etc., " agricultural environment are widely present in water and waste water
Scientific journal " the 02nd phase in 2015).Ciprofloxacin (CIP) is used as third generation fluoroquinolones, and antibacterial activity is strong, tool
There are very strong stability and hydrolysis resistance, how to be difficulty concerned by people to the purification removal containing Ciprofloxacin (CIP) waste water
Point problem.
In currently processed method, the generally existing long processing period of biological treatment, processing is not thorough, and metabolite still has suppression
The problems such as bacterium is active；Removal of the membrane processing method mainly for particulate pollutant, dissolubility organic contamination this for antibiotic
Object removal effect is general, so it is generally necessary to other technologies use in conjunction.Absorption method in terms of removing antibiotic because equally having
It is efficient high, the advantages that thorough is removed, but the generally existing adsorbent recycling of currently existing adsorbent is difficult, preparation cost is high,
The deficiencies of consumption is big.
Application for a patent for invention CN103204562A is disclosed a kind of to be polluted using antibiotics in copper sulfide Adsorption water
Waste water containing antibiotic contamination is adjusted pH to 5-9 by the method for object, realizes adsorption cleaning, processing using vulcanization copper substrate
It higher cost and cannot recycle.Patent of invention CN104108764B discloses a kind of reparation of antibiotic medicine pollutant effluents
One or more of cinnamon soil, moisture soil, red soil and black earth are mixed and cross 15-30 mesh after air-drying, in 400-600 by method
DEG C calcination 15-40min, obtains renovation agent, for the removal to antibiotic medicine in pollutant effluents.This method is forged using Low Soil Temperature
The method of burning obtains modification agent, difficult to recycle, and is not related to the resource utilization of pyrolyzing sludge residue charcoal.Invention is special
Benefit application CN106362690A discloses a kind of magnetic bio charcoal adsorbent material and preparation method thereof, which includes following
Step: (1) preparation of charcoal: the powder handled using plant biomass is raw material, and roasting obtains under anaerobic
Cavernous charcoal；(2) using ethylene glycol as dispersing agent, solid ferric iron the preparation of ferric iron precursor liquid: is added thereto
Salt then continuously adds sodium acetate and surfactant into the ethylene glycol, and disperse system, that is, ferric iron precursor liquid is formed after stirring；
(3) it solvent thermal reaction: is uniformly mixed both charcoal and ferric iron precursor liquid to obtain mixture, is placed in polytetrafluoroethylene (PTFE) water
In thermal response kettle, carries out solvent thermal reaction and obtain magnetic bio charcoal adsorbent material.Application for a patent for invention CN107096500A is public
Opened it is a kind of prepare the method for magnetic bio charcoal, magnetic bio charcoal and application using Chinese medicine slag, this method is by Chinese medicine slag and carbonic acid
After sodium pretreatment, magnetic bio charcoal is obtained through processing such as molysite dipping, high temperature anaerobic activation, washing dryings.Side of the present invention
Method have the characteristics that simple production process, raw material be easy to get, product solid-liquid it is high-efficient.In the above method, the system of magnetic bio charcoal
Standby process is complicated, and preparation cost is higher.
Summary of the invention
Problem to be solved by this invention is to overcome magnetic bio charcoal preparation process of the existing technology complicated, is prepared into
This higher problem provides the preparation method and its device and purposes of a kind of magnetic bio Carbon Materials.
Modifying agent can be introduced when usually magnetism charcoal makes, chemical modification is carried out to charcoal, just there is magnetism, the present invention does not have
It is modified, but be utilized and remain in sludge in the iron-based flocculating agent that wastewater treatment process adds, ferro element and having in sludge
Machine matter and inorganic component sufficiently merge dispersion, and after pyrolytic process processing, obtain the iron series component with good magnetism, pass through
The available magnetic material of magnetic separation.This process makes full use waste water treatment process generates the process of sludge, is considered as magnetism
The modifying process of raw material before prepared by material；The raw material that waste sludge is prepared as magnetic material is pyrolyzed obtained magnetism
Material, magnetism is preferably and cost is relatively low, without individually adding iron series precursor liquid as conventional method.
Magnetic bio Carbon Materials of the present invention be by pyrolyzing sludge, magnetic separation obtain magnetic material based on, although
The magnetic material obtained after magnetic separation has certain absorption property, but does not have fluoroquinolones antibiosis in efficient absorption solution
The performance of element, and in actual application, because granularity is smaller, it is not easy recycling.
The magnetic material obtained after magnetic separation is passed through high temperature sintering by the present invention, and the magnetic bio charcoal being prepared has prosperity
Hole make it possible to there are a large amount of capillary channel and overcome resistance between solid-liquid well, will resist through capillary action
Raw element Molecular Adsorption is fettered to pore surface, and using surface force；Due to being calcined under protective atmosphere, sludge is raw
5~10% carbons in object charcoal, are further activated in high-temperature sintering process, are evenly arranged in flourishing hole；Porous material
The metal oxide that silicon, iron, aluminium, magnesium are constituted in material has hydrophilic point, the OH after the adsorbable hydrone dissociation of metal ion-,
Oxygen atom in metal oxide then adsorbs H+, it is corresponding generate metal oxide surface hydroxy functional group Si-OH, Fe-OH,
Al-OH, Mg-OH etc.；Moreover, after high temperature anaerobic is calcined, crystal structure, surface functional group isoreactivity site increase, negative electricity
Lotus and variable charge quantity increase, so that it be made to further enhance fluoroquinolones adsorption capacity, removal rate is more than or equal to
95%.
Institute of the invention has easy regeneration feature using magnetic bio Carbon Materials, carries out thermal desorption under an inert gas, heat
Desorption temperature is 400-600 DEG C, and inert gas is nitrogen, argon gas or helium, and the desorption and regeneration time is 0.5-1h, after thermal desorption again
Raw porous material can be re-used for absorption fluoroquinolone antibiotics, to the suction of absorption fluoroquinolone antibiotics after desorption
Attached performance recovery extremely, the absorption property of the initial magnetic bio Carbon Materials of absorption property > 98%.
Concrete scheme is as follows:
A kind of preparation method of magnetic bio Carbon Materials, includes the following steps:
Step (1): sludge of sewage treatment plant is subjected to high temperature anaerobic pyrolysis and obtains sludge organism charcoal, the sewage treatment plant
Sludge is the sludge that sewage generates after iron-based flocculating agent is handled；
Step (2): the sludge organism charcoal that step (1) is obtained carries out dry method fine grinding and obtains charcoal powder；
Step (3): dry type magnetic separation is carried out to the sludge organism carbon powder that step (2) obtain, obtains magnetic material；
Step (4): the magnetic material that step (3) are obtained is conditioned and obtained particulate material after being granulated, in protective atmosphere
Lower carry out high temperature sintering, obtains sintered material；
Step (5): the sintered material furnace cooling that step (4) are obtained obtains the magnetic bio Carbon Materials of porous structure.
Further, in the step (1), the temperature of the sludge of sewage treatment plant high temperature anaerobic pyrolysis is 680-900
℃。
Further, in the step (2), charcoal powder < 100 mesh obtained after the dry method fine grinding, dry type grinding
Mode be airflow milling, ball milling or Raymond mill.
Further, in the step (3), the magnetic field strength of the dry type magnetic separation is 1500-3000Oe.
Further, in the step (4), the moisture control method of the magnetic material is to add water mixing damping, is contained after damping
Water rate is 6%-15%；
Optional, in the step (4), the prilling process is that disc granulation or roller are granulated, partial size 3-5mm；Appoint
Choosing, in the step (4), the sintering schedule of the high temperature sintering is with 3-7 DEG C/min rate from room temperature to sintering final temperature, it
20-40min is kept the temperature in the case where being sintered final temperature afterwards, sintering final temperature is 1050 DEG C -1100 DEG C；
Optional, the waste heat flue gas that sintering generates in the step (4) is back to use the step (1) high temperature Non-oxygen pyrolytic
Process；
Optional, in the step (5), the cooling rate of the furnace cooling is less than or equal to 5 DEG C/min, is cooled to room
Temperature.
The present invention also provides the devices of the preparation method with a kind of magnetic bio Carbon Materials, comprising: sludge storage
Storehouse (1), 1# conveying device (2), pyrolysis installation (3), 1# cooling device (4), 2# conveying device (5), dry method fine grinding device (6),
3# conveying device (7), concentration equipment (8), 4# conveying device (9), nonmagnetics warehouse (10), 5# conveying device (11) are magnetic
Material warehouse (12), 6# conveying device (13), damping prilling granulator (14), 7# conveying device (15), water warehouse (16), screening dress
It sets (17), 9# conveying device (19), sintering equipment (20), burner (21), 10# conveying device (22), gas cleaning plant
(23), 2# cooling device (24), 11# conveying device (25) and magnetic bio Carbon Materials warehouse (26)；
Wherein, warehouse of sludge (1) outlet is connected with 1# conveying device (2) entrance, the 1# conveying device (2)
Outlet is connected with the pyrolysis installation (3) entrance, and pyrolysis installation (3) outlet is connected with 1# cooling device (4) entrance,
The 1# cooling device (4) outlet is connected with 2# conveying device (5) entrance, the 2# conveying device (5) export with it is described
Dry method fine grinding device (6) entrance is connected, and dry method fine grinding device (6) outlet is connected with 3# conveying device (7) entrance；Institute
3# conveying device (7) outlet is stated to be connected with the concentration equipment (8) entrance；The nonmagnetics that the concentration equipment (8) magneticly elects
Matter is conveyed into the nonmagnetics warehouse (10) through the 4# conveying device (9)；
The magnetic material that the concentration equipment (8) magneticly elects is conveyed into the magnetic material through the 5# conveying device (11)
Warehouse (12)；Magnetic material warehouse (12) outlet is connected with 6# conveying device (13) entrance, the 6# conveying device
(13) outlet is connected with damping prilling granulator (14) entrance；Water in the water warehouse (16) is through the 7# conveying device
(15) the damping prilling granulator (14) is delivered into；The screening plant is arranged in damping prilling granulator (14) outlet
(17), screening plant (17) oversize delivers into the sintering equipment (20) through the 9# conveying device (19)；It is described
Sintering equipment (20) is connected with the burner (21), and making the burner (21) is the sintering equipment (20) heat supply；
The exhanst gas outlet of the sintering equipment (20) is connected with the pyrolysis installation (3), makes the sintering equipment (20) sintering waste heat cigarette
Heat source of the gas as the pyrolysis installation (3), and the gas cleaning plant is delivered into through the 10# conveying device (22)
(23) qualified discharge；Sintering equipment (20) outlet is connected with 2# cooling device (24) entrance；The 2# cooling device
(24) outlet is connected with 11# conveying device (25) entrance, 11# conveying device (25) outlet and the magnetic bio charcoal
Material warehouse (26) entrance is connected.
Further, the screening plant (17) is connected with 8# conveying device (18), makes the sieve of the screening plant (17)
Lower object is transmitted back to damping prilling granulator (14) circulation through the 8# conveying device (18) and uses；
It is optional, it is the warehouse of sludge (1), the nonmagnetics warehouse (10), the magnetic material warehouse (12), described
Water warehouse (16) or the magnetic bio Carbon Materials warehouse (26) are ordinary steel storehouse；
Optional, the 1# conveying device (2) is shaftless, uniaxially or biaxially screw conveyor；
Optional, the pyrolysis installation (3) is drum-type indirect thermal furnace；
Optional, the 1# cooling device (4) or the 2# cooling device (24) they are drum-type indirect cooling device；
Optional, the 2# conveying device (5), the 3# conveying device (7), the 4# conveying device (9), the 5# are defeated
It send device (11) or the 6# conveying device (13) is that pneumatic conveyer, belt conveyor, screw conveyor, scrapper conveyor or bucket mention
Any one in machine；
Optional, the dry method fine grinding device (6) is airslide disintegrating mill, Vertical Mill, horizontal roller mill or ball mill；
Optional, the common dry separator of the concentration equipment (8)；
Optional, the damping prilling granulator (14) is roller pelletizer or granulating disc；
Optional, the 7# conveying device (15) is common water pump；
Optional, the screening plant (17) is vibrating screen or rotary screen；
Optional, the 8# conveying device (18) is belt conveyor, screw conveyor or scrapper conveyor；
Optional, the 9# conveying device (19) is belt conveyor；
Optional, the sintering equipment (20) is indirect heating roller sintering machine；
Optional, the burner (21) is coal-fired, fuel oil or fuel gas buring furnace；
Optional, the 10# conveying device (22) is common high-temperature blower；
Optional, the gas cleaning plant (23) is common dry or wet flue gas purification system；
Optional, the 11# conveying device (25) is belt conveyor or bucket elevator.
The present invention also protects the magnetic bio being prepared with a kind of preparation method of magnetic bio Carbon Materials
Carbon Materials.
The present invention also protects the purposes of the magnetic bio Carbon Materials, for fluoroquinolones antibiosis in adsorbent solution
Element perhaps the heavy metal in adsorbent solution or is used for soil improvement.
Further, the CIP for the magnetic bio Carbon Materials being added to 1-100mg/L with the ratio of 5-15g/L is water-soluble
Under liquid conditional, CIP is adsorbed, so that the removal rate of CIP is more than or equal to 95 weight %；
Optional, after the magnetic bio Carbon Materials absorption fluoroquinolone antibiotics, it is de- that heat is carried out under an inert gas
Attached, thermal desorption temperature is 400-600 DEG C, and the desorption and regeneration time is 0.5-1h, and regenerated magnetic bio Carbon Materials are used after thermal desorption
The fluoroquinolone antibiotics in adsorbent solution, the absorption property of the initial magnetic bio Carbon Materials of absorption property > 98%；
Optional, the fluoroquinolone antibiotics are Ciprofloxacin.
The utility model has the advantages that the present invention isolates a kind of magnetic material from pyrolyzing sludge product charcoal, and it is used to prepare magnetic
Property biological carbon materials for fluoroquinolone antibiotics for example Ciprofloxacin efficient absorption remove, realize the resource of sludge organism charcoal
Change and utilize, reduces the preparation cost of adsorbent material, simple process, application is strong, with good economic efficiency and Environmental Effect
Benefit.This method can also further apply the processing of channel cleanout sludge or sea area dredged sediment.
Detailed description of the invention
Fig. 1 is a kind of preparation technology flow chart for magnetic bio Carbon Materials that the embodiment of the present invention 1 provides；
Fig. 2 is the influence diagram that the adsorption time that the embodiment of the present invention 3 provides adsorbs CIP；
Fig. 3 is the influence diagram that the additive amount that the embodiment of the present invention 4 provides adsorbs CIP.
A kind of preparation facilities structural schematic diagram for magnetic bio Carbon Materials that Fig. 4 embodiment of the present invention 5 provides；Wherein, 1.
Warehouse of sludge, 2.1# conveying device, 3. pyrolysis installations, 4.1# cooling device, 5.2# conveying device, 6. dry method fine grinding devices,
7.3# conveying device, 8. concentration equipments, 9.4# conveying device, 10. nonmagnetics warehouses, 11.5# conveying device, 12. magnetic materials
Material warehouse, 13.6# conveying device, 14. damping prilling granulators, 15.7# conveying device, 16. water warehouses, 17. screening plants,
18.8# conveying device, 19.9# conveying device, 20. sintering equipments, 21. burners, 22.10# conveying device, 23. gases are net
Makeup is set, 24.2# cooling device, 25.11# conveying device, 26. magnetic bio Carbon Materials warehouses.
Specific embodiment
Technical solution of the present invention is further elaborated below with reference to embodiment.Particular technique or item are not specified in embodiment
Part person described technology or conditions or carries out according to the literature in the art according to product description.Agents useful for same or instrument
Production firm person is not specified in device, and being can be with conventional products that are commercially available.
Embodiment 1
A kind of preparation method of magnetic bio Carbon Materials, such as Fig. 1, comprising the following steps: include the following steps: step (1):
Sludge of sewage treatment plant is subjected to high temperature anaerobic pyrolysis and obtains sludge organism charcoal；Step (2): the sludge that step (1) is obtained is raw
Object charcoal carries out dry method fine grinding and obtains charcoal powder；Step (3): dry type is carried out to the sludge organism carbon powder that step (2) obtain
Magnetic separation obtains magnetic material；Step (4): the magnetic material that step (3) are obtained is conditioned and obtained particulate material after being granulated,
High temperature sintering is carried out under protective atmosphere, obtains sintered material；Step (5): the sintered material that step (4) are obtained is cold with furnace
But, the magnetic bio Carbon Materials of porous structure are obtained.
Preferably, the waste heat flue gas that sintering generates in the step (4) is back to use the step (1) high temperature Non-oxygen pyrolytic
Process improves ability utilization efficiency.
Specifically, the temperature of the sludge of sewage treatment plant high temperature anaerobic pyrolysis is 680-900 DEG C.After the dry method fine grinding
Obtained charcoal powder < 100 mesh, the mode of dry type grinding are airflow milling, ball milling or Raymond mill.The magnetic field of the dry type magnetic separation
Intensity is 1500-3000Oe.The moisture control method of the magnetic bio Carbon Materials is to add water damping, and moisture content is 6-15 weight after damping
Measure %；The prilling process is that disc granulation or roller are granulated, partial size 3-5mm；Material particles are protected in nitrogen after the granulation
High temperature sintering is carried out under shield atmosphere, sintering schedule is with 3-7 DEG C/min rate from room temperature to sintering final temperature, and sintering final temperature is 1050
It DEG C -1100 DEG C, is cooled to room temperature after constant temperature 30min, cooling rate < 5 DEG C/min.Cooling obtains porous material, is named as SBC-
N。
Embodiment 2
Adsorption test: SBC-N prepared by embodiment 1 is added in CIP aqueous solution, in 30 DEG C of constant temperature dark shaking table
With the oscillation of 200r/min frequency, later.It sampled 0.45 μm of filter membrane and obtains sample to be tested, and carried out CIP detection.
CIP detection: the mass concentration of high performance liquid chromatography (HPLC, Hitachi L-2000, Japan) detection CIP is utilized.
Test condition: mobile phase is trichloroacetic acid, methanol and the acetonitrile (74:22:4, volume ratio) of 0.02mol/L, utilizes C-18 chromatography
Column (250mm × 4.6mm, 5-Micron 80A), post case temperature are 30 DEG C, excitation wavelength 278nm.The removal rate (r) of CIP,
Adsorbance (q in time tt) and equilibrium adsorption capacity (qe) calculation formula it is as follows:
T (h) is adsorption time, q in formulatIt (mg/g) is the adsorbance when adsorption time is t；C0、And Ct(mg/L) respectively
The mass concentration of CIP when for the concentration of initial CIP, adsorption time being t, V (L) are the volume of CIP solution；W (g) is to be added to
SBC-N mass in CIP solution.
Experiment discovery, is added to concentration according to the ratio with 10g/L by the porous material SBC-N being prepared as 100mg/
In the CIP aqueous solution of L, after vibrating 48h, CIP removal rate > 95 weight %.
The influence that 3 adsorption time of embodiment adsorbs CIP
SBC-N prepared by implementation 1 carries out adsorption test according to method in 1 is implemented, respectively 0,0.5,1,2,5,8,12,
0.45 μm of filter membrane was sampled when for 24 hours and obtains sample to be tested, carried out CIP detection.
Adsorption time is shown in Fig. 2 to the CIP impact effect adsorbed, it can be seen that after addition SBC-N, as time increases
The concentration of CIP constantly reduces in solution, after 24 hours in solution CIP residual concentration<0.5mg/L, CIP removal rate>95 weights
Measure %, it is seen that magnetic bio Carbon Materials adsorption rate prepared by the present invention is fast, quick.
After prepared magnetic bio Carbon Materials absorption fluoroquinolone antibiotics, in inert gas (nitrogen, argon gas or helium
Gas) under carry out thermal desorption, thermal desorption temperature is 400-600 DEG C, and the desorption and regeneration time is 0.5-1h, regenerated magnetism after thermal desorption
Biological carbon materials are for CIP in adsorbent solution, the absorption property of the initial magnetic bio Carbon Materials of absorption property > 98%.
The influence that 4 porous material additive amount of embodiment adsorbs CIP
By SBC-N prepared by implementation 1 with 5.0,7.5,10.0,12.5,15.0,20.0,25.0,30.0,40.0g/L adds
Dosage is added separately to the CIP aqueous solution of 10mg/L, in 30 DEG C of constant temperature dark shaking table for 24 hours with the oscillation of 200r/min frequency
Sampling filtering afterwards carries out CIP detection, the influence that research SBC-N additive amount adsorbs CIP.From figure 3, it can be seen that with SBC-N
The increase of additive amount, CIP removal rate are continuously increased；When additive amount is increased to 5g/L, to the removal rate of CIP to reach 100%,
Adsorption capacity corresponding to it is 2mg/g, it is seen then that magnetic bio Carbon Materials large amount of adsorption prepared by the present invention adsorbs CIP
Excellent effect.
Magnetic bio Carbon Materials prepared by the present invention, it is water-soluble with the CIP that the ratio of 5-15g/L is added to 1-100mg/L
Under liquid conditional, CIP is adsorbed, so that the removal rate of CIP is more than or equal to 95 weight %.
From embodiment 3 and embodiment 4 as can be seen that magnetic bio Carbon Materials prepared by the present invention have stronger absorption
Performance, when being adsorbed capillarity principle and metal oxide hydrophilic point similar to CIP property in view of fluoroquinolone antibiotics
Position absorption principle is identical, and those skilled in the art are it is contemplated that magnetic bio Carbon Materials are to fluoquinolone prepared by the present invention
Class antibiotic all has adsorption effect, and is more than or equal to 95 weight % to the removal rate of fluoroquinolone antibiotics, while liquid can
With for the heavy metal in adsorbent solution, or it is used for soil improvement.
Embodiment 5
A kind of preparation facilities of magnetic bio Carbon Materials, as shown in Figure 4, comprising: warehouse of sludge 1,1# conveying device 2, heat
Solve device 3,1# cooling device 4,2# conveying device 5, dry method fine grinding device 6,3# conveying device 7, concentration equipment 8,4# conveying dress
Set 9, nonmagnetics warehouse 10,5# conveying device 11, magnetic material warehouse 12,6# conveying device 13, damping prilling granulator 14,7#
Conveying device 15, water warehouse 16, screening plant 17,9# conveying device 19, sintering equipment 20, burner 21,10# conveying device
22, gas cleaning plant 23,2# cooling device 24,11# conveying device 25 and magnetic bio Carbon Materials warehouse 26；
Wherein, the warehouse of sludge 1 outlet is connected with 2 entrance of 1# conveying device, the 1# conveying device 2 export and
3 entrance of pyrolysis installation is connected, and the outlet of pyrolysis installation 3 is connected with 4 entrance of 1# cooling device, the cooling dress of the 1#
It sets 4 outlets to be connected with 5 entrance of 2# conveying device, the outlet of 2# conveying device 5 and the 6 entrance phase of dry method fine grinding device
Even, the outlet of dry method fine grinding device 6 is connected with 7 entrance of 3# conveying device；The outlet of 3# conveying device 7 and the magnetic
8 entrance of screening device is connected；The namagnetic substance that the concentration equipment 8 magneticly elects is conveyed into described non-through the 4# conveying device 9
Magnetic material warehouse 10；
The magnetic material that the concentration equipment 8 magneticly elects is conveyed into the magnetic material warehouse through the 5# conveying device 11
12；The outlet of magnetic material warehouse 12 is connected with 13 entrance of 6# conveying device, the outlet of 6# conveying device 13 and institute
14 entrance of damping prilling granulator is stated to be connected；Water in the water warehouse 16 delivers into the damping through the 7# conveying device 15
Prilling granulator 14；The screening plant 17 is arranged in the outlet of damping prilling granulator 14, and 17 oversize of screening plant is through institute
It states 9# conveying device 19 and delivers into the sintering equipment 20；The sintering equipment 20 is connected with the burner 21, makes institute
Stating burner 21 is 20 heat supply of sintering equipment；The exhanst gas outlet of the sintering equipment 20 is connected with the pyrolysis installation 3,
Make heat source of the 20 sintering waste heat flue gas of sintering equipment as the pyrolysis installation 3, and is conveyed through the 10# conveying device 22
Into 23 qualified discharge of gas cleaning plant；The outlet of sintering equipment 20 is connected with 24 entrance of 2# cooling device；
The outlet of 2# cooling device 24 is connected with 25 entrance of 11# conveying device, the outlet of 11# conveying device 25 and the magnetic
Property 26 entrances of biological carbon materials warehouses be connected.
Preferably, the screening plant 17 is connected with 8# conveying device 18, makes the screenings of the screening plant 17 through institute
It states 8# conveying device 18 and is transmitted back to the circulation of damping prilling granulator 14 use.
Specifically, warehouse of sludge 1, nonmagnetics warehouse 10, magnetic bio charcoal warehouse 12, water warehouse 16 and porous material storage
Storehouse 26 is ordinary steel storehouse；
1# conveying device 2 is shaftless, uniaxially or biaxially screw conveyor；
Pyrolysis installation 3 is drum-type indirect thermal furnace；
1# cooling device 4 and 2# cooling device 24 are drum-type indirect cooling device；
2# conveying device 5,3# conveying device 7,4# conveying device 9,5# conveying device 11 and 6# conveying device 13 are strength
Conveyer, belt conveyor, screw conveyor, scrapper conveyor or bucket elevator；
Dry method fine grinding device 6 is airslide disintegrating mill, Vertical Mill, horizontal roller mill or ball mill；
The common dry separator of concentration equipment 8；
Damping prilling granulator 14 is roller pelletizer or granulating disc；
7# conveying device 15 is common water pump；
Screening plant 17 is vibrating screen or rotary screen；
8# conveying device 18 is belt conveyor, screw conveyor, scrapper conveyor；
9# conveying device 19 is belt conveyor；
Sintering equipment 20 is indirect heating roller sintering machine；
Burner 21 is coal-fired, fuel oil or fuel gas buring furnace；
10# conveying device 22 is common high-temperature blower；
Gas cleaning plant 23 is common dry or wet flue gas purification system；
11# conveying device 25 is belt conveyor or bucket elevator.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, it can be combined in any appropriate way.In order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (10)
1. a kind of preparation method of magnetic bio Carbon Materials, includes the following steps:
Step (1): sludge of sewage treatment plant is subjected to high temperature anaerobic pyrolysis and obtains sludge organism charcoal, the sludge of sewage treatment plant
The sludge generated after iron-based flocculating agent is handled for sewage；
Step (2): the sludge organism charcoal that step (1) is obtained carries out dry method fine grinding and obtains charcoal powder；
Step (3): dry type magnetic separation is carried out to the sludge organism carbon powder that step (2) obtain, obtains magnetic material；
Step (4): the magnetic material that step (3) are obtained is conditioned and obtained particulate material after being granulated, under protective atmosphere into
Row high temperature sintering, obtains sintered material；
Step (5): the sintered material furnace cooling that step (4) are obtained obtains the magnetic bio Carbon Materials of porous structure.
2. a kind of preparation method of magnetic bio Carbon Materials according to claim 1, it is characterised in that: the step (1)
In, the temperature of the sludge of sewage treatment plant high temperature anaerobic pyrolysis is 680-900 DEG C.
3. a kind of preparation method of magnetic bio Carbon Materials according to claim 1, it is characterised in that: the step (2)
In, charcoal powder < 100 mesh obtained after the dry method fine grinding, the mode of dry type grinding is airflow milling, ball milling or Raymond mill.
4. a kind of preparation method of magnetic bio Carbon Materials according to claim 1, it is characterised in that: the step (3)
In, the magnetic field strength of the dry type magnetic separation is 1500-3000Oe.
5. a kind of preparation method of magnetic bio Carbon Materials according to claim 1, it is characterised in that: the step (4)
In, the moisture control method of the magnetic material is to add water mixing damping, and moisture content is 6-15 weight % after damping；
Optional, in the step (4), the prilling process is that disc granulation or roller are granulated, partial size 3-5mm；
Optional, in the step (4), the sintering schedule of the high temperature sintering is with 3-7 DEG C/min rate from room temperature to sintering
Final temperature, keeps the temperature 20-40min in the case where being sintered final temperature later, and sintering final temperature is 1050 DEG C -1100 DEG C；
Optional, the waste heat flue gas that sintering generates in the step (4) is back to use the step (1) high temperature Non-oxygen pyrolytic mistake
Journey；
Optional, in the step (5), the cooling rate of the furnace cooling is less than or equal to 5 DEG C/min, is cooled to room temperature.
6. using a kind of device of the preparation method of magnetic bio Carbon Materials of any of claims 1-5, comprising: dirty
Mud warehouse (1), 1# conveying device (2), pyrolysis installation (3), 1# cooling device (4), 2# conveying device (5), dry method fine grinding device
(6), 3# conveying device (7), concentration equipment (8), 4# conveying device (9), nonmagnetics warehouse (10), 5# conveying device (11),
Magnetic material warehouse (12), 6# conveying device (13), damping prilling granulator (14), 7# conveying device (15), water warehouse (16), sieve
Separating device (17), 9# conveying device (19), sintering equipment (20), burner (21), 10# conveying device (22), gas purification
Device (23), 2# cooling device (24), 11# conveying device (25) and magnetic bio Carbon Materials warehouse (26)；
Wherein, warehouse of sludge (1) outlet is connected with 1# conveying device (2) entrance, 1# conveying device (2) outlet
It is connected with the pyrolysis installation (3) entrance, pyrolysis installation (3) outlet is connected with 1# cooling device (4) entrance, described
1# cooling device (4) outlet is connected with 2# conveying device (5) entrance, 2# conveying device (5) outlet and the dry method
Fine grinding device (6) entrance is connected, and dry method fine grinding device (6) outlet is connected with 3# conveying device (7) entrance；The 3#
Conveying device (7) outlet is connected with the concentration equipment (8) entrance；The namagnetic substance warp that the concentration equipment (8) magneticly elects
The 4# conveying device (9) is conveyed into the nonmagnetics warehouse (10)；
The magnetic material that the concentration equipment (8) magneticly elects is conveyed into the magnetic material warehouse through the 5# conveying device (11)
(12)；Magnetic material warehouse (12) outlet is connected with 6# conveying device (13) entrance, the 6# conveying device (13)
Outlet is connected with damping prilling granulator (14) entrance；Water in the water warehouse (16) is defeated through the 7# conveying device (15)
It is fed into the damping prilling granulator (14)；
The damping prilling granulator (14), which exports, is arranged the screening plant (17), described in screening plant (17) the oversize warp
9# conveying device (19) delivers into the sintering equipment (20)；The sintering equipment (20) and the burner (21) phase
Even, making the burner (21) is the sintering equipment (20) heat supply；The exhanst gas outlet of the sintering equipment (20) with it is described
Pyrolysis installation (3) is connected, and makes heat source of the sintering equipment (20) the sintering waste heat flue gas as the pyrolysis installation (3), and pass through
The 10# conveying device (22) delivers into the gas cleaning plant (23) qualified discharge；Sintering equipment (20) outlet
It is connected with 2# cooling device (24) entrance；2# cooling device (24) outlet and 11# conveying device (25) entrance
It is connected, 11# conveying device (25) outlet is connected with magnetic bio Carbon Materials warehouse (26) entrance.
7. a kind of device of the preparation method according to claim 6 with magnetic bio Carbon Materials, it is characterised in that: institute
It states screening plant (17) to be connected with 8# conveying device (18), makes the screenings of the screening plant (17) through the 8# conveying device
(18) damping prilling granulator (14) circulation is transmitted back to use；
Optional, the warehouse of sludge (1), the nonmagnetics warehouse (10), the magnetic material warehouse (12), water storage
Storehouse (16) or the magnetic bio Carbon Materials warehouse (26) are ordinary steel storehouse；
Optional, the 1# conveying device (2) is shaftless, uniaxially or biaxially screw conveyor；
Optional, the pyrolysis installation (3) is drum-type indirect thermal furnace；
Optional, the 1# cooling device (4) or the 2# cooling device (24) they are drum-type indirect cooling device；
Optional, the 2# conveying device (5), the 3# conveying device (7), the 4# conveying device (9), 5# conveying dress
It sets (11) or the 6# conveying device (13) is in pneumatic conveyer, belt conveyor, screw conveyor, scrapper conveyor or bucket elevator
Any one；
Optional, the dry method fine grinding device (6) is airslide disintegrating mill, Vertical Mill, horizontal roller mill or ball mill；
Optional, the common dry separator of the concentration equipment (8)；
Optional, the damping prilling granulator (14) is roller pelletizer or granulating disc；
Optional, the 7# conveying device (15) is common water pump；
Optional, the screening plant (17) is vibrating screen or rotary screen；
Optional, the 8# conveying device (18) is belt conveyor, screw conveyor or scrapper conveyor；
Optional, the 9# conveying device (19) is belt conveyor；
Optional, the sintering equipment (20) is indirect heating roller sintering machine；
Optional, the burner (21) is coal-fired, fuel oil or fuel gas buring furnace；
Optional, the 10# conveying device (22) is common high-temperature blower；
Optional, the gas cleaning plant (23) is common dry or wet flue gas purification system；
Optional, the 11# conveying device (25) is belt conveyor or bucket elevator.
8. with a kind of magnetism that the preparation method of magnetic bio Carbon Materials is prepared of any of claims 1-5
Biological carbon materials.
9. the purposes of magnetic bio Carbon Materials according to any one of claims 8, for fluoroquinolone antibiotics in adsorbent solution, or
Heavy metal in adsorbent solution, or it is used for soil improvement.
10. the purposes of magnetic bio Carbon Materials according to claim 9, which is characterized in that by the magnetic bio raw material of wood-charcoal
Material is added under the CIP aqueous solution conditional of 1-100mg/L with the ratio of 5-15g/L, CIP is adsorbed, so that the removal rate of CIP is big
In equal to 95 weight %；
Optional, after the magnetic bio Carbon Materials absorption fluoroquinolone antibiotics, thermal desorption is carried out under an inert gas, heat
Desorption temperature is 400-600 DEG C, and the desorption and regeneration time is 0.5-1h, and regenerated magnetic bio Carbon Materials are for adsorbing after thermal desorption
Fluoroquinolone antibiotics in solution, the absorption property of the initial magnetic bio Carbon Materials of absorption property > 98%；
Optional, the fluoroquinolone antibiotics are Ciprofloxacin.
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| CN201910004100.4A CN109621897B (en) | 2019-01-03 | 2019-01-03 | Preparation method of magnetic biochar material, device and application thereof |
| PCT/CN2019/127270 WO2020140779A1 (en) | 2019-01-03 | 2019-12-23 | Preparation method for magnetic biochar material, device therefor and use thereof |
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