CN110075802A - The active carbon and its synthetic method of a kind of load of ferriferous oxide and application - Google Patents
The active carbon and its synthetic method of a kind of load of ferriferous oxide and application Download PDFInfo
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- CN110075802A CN110075802A CN201910471400.3A CN201910471400A CN110075802A CN 110075802 A CN110075802 A CN 110075802A CN 201910471400 A CN201910471400 A CN 201910471400A CN 110075802 A CN110075802 A CN 110075802A
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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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/34—Biological treatment of water, waste water, or sewage characterised by the microorganisms used
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Abstract
The invention belongs to water treatment field, active carbon and its synthetic method and the application of a kind of ferriferous oxide load are disclosed.Synthetic method is ultrasonically treated the following steps are included: active carbon is immersed in the aqueous solution of source of iron, is then evaporated, roast the active carbon loaded to get ferriferous oxide.The synthetic method bring the load of Fe, in the generation of Fe-O-C key and duct filamentary structure formation；The active carbon has big specific surface area, and organic pollutant is more fully adsorbed in active carbon duct, and the extracellular microbial exoelectron delivery rate of apposition growth is accelerated, and the formation of biomembrane is promoted.The present invention does not terminate in the disinfection by-products and pathogenic microorganisms reduced in output water, even more has the function of inhibiting disinfection by-products in subsequent tap water pipe network to generate and pathogenic microorganisms regrowth.
Description
Technical field
The invention belongs to water treatment field, in particular to the active carbon of a kind of ferriferous oxide load and its synthetic method with answer
With.
Background technique
In recent years, the microorganism problem of potable water network is gradually by social concerns.In general, the faucet of resident
Water compares the output water of waterworks, and due to the regrowth of microorganism in pipe network, water quality obviously deteriorates.In order to reduce this harm,
Introduce chlorhexidine-containing disinfectant in 20th century because its cost is relatively low and remains that certain residual chlorine concentration is able in entire pipe network
Continuous sterilization.However chlorhexidine-containing disinfectant can be reacted with the natural organic matter in water, generate a series of harmful disinfection by-products examples
Such as haloform and halogen acetic acid, carcinogenesis is generated to human body.
Recently, the conditioned pathogen of raised growth such as Mycobacterium avium in potable water network,
Legionella pneumophila and Hartmanella vermiformis etc. becomes the new focus of public attention.It is different
In the enteric microorganism easily killed by chlorhexidine-containing disinfectant, conditioned pathogen can survive well in pipe network, expand and breed very
To under very high decontaminant concentration because its with a series of advantage include biomembrane easy to form, generate it is a large amount of extracellular
Polymer, anti-oligotrophic etc..
To improve drinking water quality, advanced treating means quilt of the ozone-biological active carbon group technology as drinking water plant
It is widely applied.Ozone it is verified that can with oxidation sterilizing by-product presoma, removal Taste and odor compounds, inactivation pathogenic microorganisms and
The biodegradability of organic matter is improved, while facilitation is played to the microbial metabolic activity of subsequent bio active carbon.Biology
Active carbon can remove removal organic polluter and disinfection by-products presoma significantly, while retain most of pathogenic bacteria.
However there is also certain defects, such as ozone oxidation organic matter process meeting shape for ozone-biological active carbon combination technique
The disinfection by-products presoma of Cheng Xin.The biomembrane to fall off while biological activated carbon efficiently removes removal organic polluter and dissolution
Property microbial metabolic products can also serve as disinfection by-products presoma, the latter is even more that can do harm to huamn body.In addition, de-
Containing a large amount of invasive organism in the biomembrane fallen, more mature biofilm structure plays protective effect to microorganism,
It is difficult to be inactivated by chlorhexidine-containing disinfectant after entering pipe network, and is regenerated length.Although the most of microbe of tap water output water exists
It is inactivated after chlorination, but the pathogenic microorganisms after pipe network transmission & distribution in water,tap is not controlled effectively
System, disinfection by-products still will continue to generate.If transition metal oxide can be loaded to activated carbon surface to be modified, formed
Metal oxygen key enhances the complexing and extracellular microbial exoelectron delivery rate of organic matter, and allows the biofilm structure of activated carbon surface
It is more excellent, improve organic matter, biomembrane form and the biological community structure of active carbon water outlet, and then ensure in subsequent pipe network
Water quality stability, then can solve the problems, such as the disinfection by-products and pathogenic microorganisms of water,tap simultaneously.
Summary of the invention
In order to overcome the shortcomings and deficiencies of the prior art described above, the primary purpose of the present invention is that providing a kind of ferriferous oxide
The synthetic method of the active carbon of load.This method is using common active carbon as matrix, by being impregnated into source of iron, being evaporated, forge
Burn three steps synthesis target novel absorbent charcoal.
Another object of the present invention is to provide the active carbon of the ferriferous oxide load of above method preparation, above-mentioned synthesis side
Method bring the load of Fe, in the generation of Fe-O-C key and duct filamentary structure formation；The active carbon has big ratio
Surface area, organic pollutant are more fully adsorbed in active carbon duct, the extracellular microbial exoelectron delivery rate of apposition growth
It is accelerated, the formation of biomembrane is promoted.
A further object of the present invention is to provide the active carbons of above-mentioned ferriferous oxide load, and tap water pipe network to be inhibited to go out
The application of disinfection by-products and pathogenic microorganisms in water, the common active carbon of this inhibitory effect do not have.
The purpose of the present invention is realized by following proposal:
A kind of synthetic method of the active carbon of ferriferous oxide load, comprising the following steps: active carbon is immersed in source of iron
In aqueous solution, then ultrasonic treatment is evaporated, roasts the active carbon loaded to get ferriferous oxide.
The active carbon be one of cocoanut active charcoal, coaly activated carbon, wood activated charcoal, activated carbon from bamboo, it is excellent
It is selected as cocoanut active charcoal；
The active carbon diameter is 0.5~3mm, preferably 1.2mm；
The source of iron is Iron trichloride hexahydrate (FeCl3·6H2O) He Jiushui ferric nitrate (FeNO3·9H2One of O),
Preferably Iron trichloride hexahydrate (FeCl3·6H2O)；
The concentration of the source of iron aqueous solution is 15~25g/L, preferably 20g/L.
The dosage of the active carbon and source of iron aqueous solution meets: the corresponding iron for being immersed in (2~4) mL of the active carbon of every 1g
In the aqueous solution of source, the active carbon correspondence of preferably every 1g is immersed in the source of iron aqueous solution of 3mL；
The ultrasonic treatment refers to be ultrasonically treated 0.5~1.5 hour in 300W power, preferably in 300W power ultrasound
Processing 1 hour.Ultrasonic treatment is chiefly to facilitate molysite and is dispersed in the hole of active carbon prosperity, is conducive to filamental knot in duct
The formation of structure ferriferous oxide, the structure is essential, significantly increases the site of organic matter absorption and attached growth of microorganisms, and
Improve extracellular microbial exoelectron delivery rate.
Described be evaporated refers to and is evaporated at 75~95 DEG C；
The heating rate of the roasting is less than 20 DEG C/min, preferably 5 DEG C/min；The maturing temperature be 200~
400 DEG C, preferably 300 DEG C；The calcining time is 0.5~2h, preferably 1h；
The active carbon further includes a pre-treatment step, pretreated mesh before being impregnated into the aqueous solution of source of iron
There are two, first is that removal impurity, second is that activated carbon surface group, surface Carbon Materials and iron oxygen more conducively in synthesis process
The formation of compound bonding, Fe-O-C key is essential.Pre-treatment step is specifically includes the following steps: active carbon is successively immersed in
It in alkaline aqueous solution and acidic aqueous solution, is then washed with water, is dried for standby；
The alkaline aqueous solution is preferably the sodium hydrate aqueous solution of 50~150g/L, preferably the hydroxide of 100g/L
Sodium water solution；The time impregnated in alkaline aqueous solution is 0.5~2h；It is preferably first used after alkaline aqueous solution immersion
It is placed in acidic aqueous solution and impregnates again after water washing.
The acidic aqueous solution is preferably the HNO that concentration is 5%~15% (v/v)3Aqueous solution, preferably 10% (v/
V) HNO3Aqueous solution；The time impregnated in acidic aqueous solution is 0.5~2h；
The drying is preferably dried at 100~200 DEG C, preferably 160 DEG C drying.
A kind of active carbon of ferriferous oxide load prepared by the above method.Ferriferous oxide prepared by the above method
The active carbon of load is still the solid particle of black, and appearance and common active carbon do not have difference；Its microstructure is activity
Filamental ferriferous oxide structure is formd in the duct of charcoal prosperity.Iron is entered in the structural framework of activated carbon surface and is formed
Fe-O-C key.The active carbon of ferriferous oxide load has bigger specific surface area, and organic pollutant is more fully adsorbed on work
In property charcoal duct, the extracellular microbial exoelectron delivery rate of apposition growth is accelerated.
Disinfection by-product of the active carbon of above-mentioned ferriferous oxide load in inhibiting drinking water and in tap water pipe network water outlet
Application in object and pathogenic microorganisms.
The disinfection by-products may include haloform and halogen acetic acid；The pathogenic microorganisms includes Shi Fei legion bar
Bacterium, mycobacterium avium, naegleria fowleri worm etc..
The present invention compared with the existing technology, have the following advantages and the utility model has the advantages that
(1) active carbon of ferriferous oxide of the invention load has higher removal rate to disinfection by-products presoma.
(2) active carbon of the invention has more excellent pore structure, large specific surface area, formation filamental knot in duct
Structure, active component are greatly exposed to activated carbon surface, considerably increase the adsorption site of organic matter.
(3) of the invention to generate heavy metal pollution in use.
(4) microbial metabolic activity of activated carbon surface of the invention is higher, and biofilm structure is more flourishing.
(5) active carbon of the invention discharges less microorganism and biomembrane during biodegradable organic pollutant
Scale scale is smaller.
(6) the active carbon water outlet of ferriferous oxide load has less organic matter and disinfection by-products presoma, and
Suspended state biomembrane is smaller in water outlet water body, it is easier to be inactivated by disinfectant, such water body chlorination enters defeated
After pipe network, due to organic matter, the limitation of the scarcity of disinfection by-products presoma and biomembrane size, disinfection by-products is generated
It is able to continue inhibition with pathogenic microorganisms regrowth.Therefore, the present invention does not terminate in the disinfection by-products and cause reduced in output water
Sick microorganism even more has the function of inhibiting disinfection by-products in subsequent tap water pipe network to generate and pathogenic microorganisms regrowth.
Detailed description of the invention
Fig. 1 is the SEM figure of the Fe/CAC and raw material CAC that are prepared in embodiment 1.
Fig. 2 is the N of the Fe/CAC and raw material CAC that prepare in embodiment 12Adsorption/desorption isotherms.
Fig. 3 is the XRD spectra of the Fe/CAC and raw material CAC that prepare in embodiment 1.
Fig. 4 is the infrared spectrogram of the Fe/CAC and raw material CAC that prepare in embodiment 1.
Fig. 5 is the O1s XPS spectrum figure of the Fe/CAC and raw material CAC that prepare in embodiment 1.
Under the conditions of Fig. 6 is the Fe/CAC and control activity high-area carbon (common CAC) prepared using embodiment 1, pipe network is simulated
The haloform and halogen acetic acid of water outlet generate situation map.
Under the conditions of Fig. 7 is the Fe/CAC and control activity high-area carbon (common CAC) prepared using embodiment 1, pipe network is simulated
The conditioned pathogen situation map of water outlet.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Agents useful for same can routinely be bought unless otherwise specified from market in embodiment.
Embodiment 1
The synthetic method of the cocoanut active charcoal Fe/CAC of ferriferous oxide load of the present invention, comprising the following steps:
(1) cocoanut active charcoal (CAC) of average grain diameter 1.2mm is immersed into 100g/L sodium hydroxide solution (NaOH) 1 hour；
(2) it takes out above-mentioned cocoanut active charcoal to be washed with deionized, immerses the aqueous solution of nitric acid of volumetric concentration 10% later
(HNO3) 1 hour；
(3) it takes out above-mentioned cocoanut active charcoal to be washed with deionized repeatedly 5 times, be dried for standby for 160 DEG C in an oven.
(4) by Iron trichloride hexahydrate (FeCl3·6H2O it) dissolves in deionized water, forms the solution A that concentration is 20g/L；
(5) solution A and pretreated cocoanut active charcoal are mixed with ratio 3mL:1.0g, 300W power ultrasonic treatment 1
Hour, 85 DEG C of heating water baths, until being evaporated liquid；
(6) by the cocoanut active charcoal after above-mentioned water bath method in Muffle furnace 300 DEG C roast 1 hour, obtained after Temperature fall
Obtain the novel cocoanut active charcoal Fe/CAC of ferriferous oxide load finally.
Fig. 1 is the SEM figure of the Fe/CAC and raw material CAC that are prepared in embodiment 1.As can be seen from the figure Fe/CAC
Partial size itself is about 1~2mm, and has more flourishing pore structure, and the structure of filamental is formd in duct.
Fig. 2 is the N of the Fe/CAC and raw material CAC that prepare in embodiment 12Adsorption/desorption isotherms are measured by BET,
The specific surface area of raw material CAC is 641.09m2g-1, Fe/CAC is with bigger specific surface area, about 680m2g-1.Pass through EDS energy
The surface Fe content of spectrum analysis, Fe/CAC is 3.33wt%, and its body phase iron content is about 1.25wt%, is shown Fe a large amount of
Point is exposed on activated carbon surface.
Fig. 3 is the XRD spectra of the Fe/CAC and raw material CAC that prepare in embodiment 1.As can be seen from the figure Fe/CAC table
The ferriferous oxide of face load is mainly with Fe2O3Crystal form exist, carbonizable substance mainly in the form of graphitized carbon exist.
Fig. 4 is the infrared spectrogram of the Fe/CAC and raw material CAC that prepare in embodiment 1, when coconut activated carbon surface is negative
After carrying iron, there is 544cm-1And 474cm-1Two new peaks are Fe2O3In Fe-O key characteristic peak, with above-mentioned XRD result
It is consistent.In addition, also newly there is 1701cm-1Locate characteristic peak, represents the C-O key in carboxylic acid and ketone structure.Represent CH2It is asymmetric
With the 2924cm of midplane extrusion vibration-1And 2860cm-1Locating peak intensity reduces, and illustrates that the C-O-H key of its activated carbon surface is increased
Add.3480cm-1Place's hydroxyl is moved to 3425cm-1, illustrate other than C-O-H, iron load also introduces Fe-O-H, thus causes
The movement of hydroxyl peak.
Fig. 5 is the O1s XPS spectrum figure of the Fe/CAC and raw material CAC that prepare in embodiment 1.As can be seen from the figure Fe/
The iron species on the surface CAC in conjunction with activated carbon surface, and further demonstrate depositing for Fe-O-Fe and Fe-O-H with Fe-O-C key
?.
Application Example
The water outlet of sand filter is obtained from waterworks, first progress ozone treatment, subsequently enter the fixation of carrying active charcoal
In bed, the residence time is 30 minutes.After the active carbon processing that water body is loaded through ferriferous oxide, chlorination is carried out, disinfectant is
Sodium hypochlorite subsequently enters chlorine reaction tank, and the residence time is 4 hours.The water outlet of chlorine reaction tank enters Simulative tap water pipe network immediately.
(ozone treatment and the process conditions of active carbon processing are the common parameter in practical waterworks, and ozone adds dosage and be
1.0mg/L, the residence time of active carbon and filtering velocity be respectively 30 minutes and 10 meters per hour.)
Under the conditions of Fig. 6 is the Fe/CAC and control activity high-area carbon (common CAC) prepared using embodiment 1, pipe network is simulated
The haloform and halogen acetic acid of water outlet generate situation (test method is U.S. EPA standard method) figure.As shown in fig. 6, in CAC
Under the use of Fe/CAC, the haloform concentration of simulation pipe network water outlet is respectively 8.46ug/L and 2.15ug/L, and halogen acetic acid is dense
Degree is respectively 28.45ug/L and 10.55ug/L.Obviously, the active carbon loaded using ferriferous oxide prepared by the present invention, pipe network are gone out
Haloform and halogen acetic acid in water are obviously suppressed, and reduce the risk of disinfection by-products in water,tap.
Under the conditions of Fig. 7 is the Fe/CAC and control activity high-area carbon (common CAC) prepared using embodiment 1, pipe network is simulated
The conditioned pathogen situation map of water outlet.As shown in fig. 7, belonging in level, legion in the case of the Fe/CAC prepared using embodiment 1
Pseudomonas, every milliliter of water body of branch Pseudomonas and Nai Geli Entamoeba gene copy number be reduced to 1.18,0.97 and 0 respectively
log.And have in pathogenic kind level from determining, legionella pneumophilia, mycobacterium avium and naegleria fowleri
Worm is inactivated.In addition, the burst size of Fe/CAC iron is considerably less in entire reaction, it is lower than 0.1mg L-1And iron sheet
Body is nontoxic.Therefore, Fe/CAC effectively inhibits disinfection by-products and pathogenic microorganisms in pipe network, has ensured water,tap
Water quality safety.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of synthetic method of the active carbon of ferriferous oxide load, it is characterised in that the following steps are included: active carbon is impregnated
In the aqueous solution of source of iron, then ultrasonic treatment is evaporated, roasts the active carbon loaded to get ferriferous oxide.
2. the synthetic method of the active carbon of ferriferous oxide load according to claim 1, it is characterised in that:
The active carbon is one of cocoanut active charcoal, coaly activated carbon, wood activated charcoal, activated carbon from bamboo；
The source of iron is one of Iron trichloride hexahydrate and nine water ferric nitrates.
3. the synthetic method of the active carbon of ferriferous oxide load according to claim 1, it is characterised in that:
The active carbon is cocoanut active charcoal；
The source of iron is Iron trichloride hexahydrate.
4. the synthetic method of the active carbon of ferriferous oxide load according to claim 1 or 2, it is characterised in that:
The concentration of the source of iron aqueous solution is 15~25g/L；
The dosage of the active carbon and source of iron aqueous solution meets: the corresponding source of iron water for being immersed in (2~4) mL of the active carbon of every 1g
In solution.
5. the synthetic method of the active carbon of ferriferous oxide load according to claim 1 or 2, it is characterised in that:
The concentration of the source of iron aqueous solution is 20g/L；
The dosage of the active carbon and source of iron aqueous solution meets: the corresponding source of iron aqueous solution for being immersed in 3mL of the active carbon of every 1g
In.
6. the synthetic method of the active carbon of ferriferous oxide load according to claim 1 or 2, it is characterised in that:
The ultrasonic treatment refers to be ultrasonically treated 0.5~1.5 hour in 300W power；
Described be evaporated refers to and is evaporated at 75~95 DEG C；
The heating rate of the roasting is less than 20 DEG C/min；The maturing temperature is 200~400 DEG C；When the described roasting
Between be 0.5~2h.
7. the synthetic method of the active carbon of ferriferous oxide load according to claim 1, it is characterised in that:
The active carbon further includes a pre-treatment step before being impregnated into the aqueous solution of source of iron, and pre-treatment step is specific
The following steps are included: active carbon is successively immersed in alkaline aqueous solution and acidic aqueous solution, then it is washed with water, dries standby
With；
The alkaline aqueous solution be 50~150g/L sodium hydrate aqueous solution, it is described impregnated in alkaline aqueous solution when
Between be 0.5~2h；
The acidic aqueous solution is the HNO that volumetric concentration is 5%~15%3Aqueous solution, it is described to be impregnated in acidic aqueous solution
Time be 0.5~2h；
The drying is to dry at 100~200 DEG C.
8. a kind of active carbon for the ferriferous oxide load that methods described in any item according to claim 1~7 are prepared.
9. the active carbon of ferriferous oxide load according to claim 8 is in inhibiting drinking water and in tap water pipe network water outlet
Disinfection by-products and pathogenic microorganisms in application.
10. the active carbon of ferriferous oxide load according to claim 9 is in inhibiting drinking water and tap water pipe network is discharged
In disinfection by-products and pathogenic microorganisms in application, it is characterised in that:
The disinfection by-products includes haloform and halogen acetic acid；The pathogenic microorganisms includes bacillus legionnaires,pneumophila, bird
Type mycobacteria, naegleria fowleri worm.
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| CN114455699A (en) * | 2021-12-24 | 2022-05-10 | 清华大学 | Iron-carbon composite carrier and application thereof |
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| CN111547790A (en) * | 2020-06-22 | 2020-08-18 | 河南师范大学 | Preparation method of biomass water treatment environment functional material |
| CN113262758A (en) * | 2021-06-02 | 2021-08-17 | 重庆交通大学 | Preparation method and application of trivalent manganese modified biomass charcoal |
| CN114455699A (en) * | 2021-12-24 | 2022-05-10 | 清华大学 | Iron-carbon composite carrier and application thereof |
| CN114455699B (en) * | 2021-12-24 | 2023-03-14 | 清华大学 | Iron-carbon composite carrier and application thereof |
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