CN104961228A - Magnetic sludge carbon biological filler with core-at-shell structure and preparation method and application thereof - Google Patents

Magnetic sludge carbon biological filler with core-at-shell structure and preparation method and application thereof Download PDF

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Publication number
CN104961228A
CN104961228A CN201510383999.7A CN201510383999A CN104961228A CN 104961228 A CN104961228 A CN 104961228A CN 201510383999 A CN201510383999 A CN 201510383999A CN 104961228 A CN104961228 A CN 104961228A
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sludge
magnetic
shell
core
carbon
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CN104961228B (en
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熊亚
伍志趼
田双红
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Sun Yat Sen University
National Sun Yat Sen University
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National Sun Yat Sen University
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00Technologies for wastewater treatment
    • Y02W10/10Biological treatment of water, waste water, or sewage

Abstract

The invention discloses magnetic sludge carbon biological filler with a core-at-shell structure and preparation method and application thereof. The magnetic sludge carbon biological filler is prepared by using Fe3O4 magnetic microsphere as a magnetic core, iron-containing sludge as an intermediate layer raw material and common sludge or zinc-containing sludge (preferred) as a shell raw material, adopting a repetitive impregnation-drying method to sequentially wrap the intermediate layer raw material and the shell raw material on the Fe3O4 magnetic microsphere to form a precursor of the core-at-shell structure, and then performing pyrolysis and after-treatment. Since the magnetic material is used as the core and the sludge carbon is used as the shell material, the prepared magnetic sludge carbon biological filler with the core-at-shell structure not only can solve the problem that a powder magnetic material is difficult to separate, and can also solve the problem that ferrite used as a magnetic matrix is corroded by microorganisms; the specific surface of the porous sludge carbon in a shell layer is large, a magnetic environment for growth can be provided for more microorganisms, the metabolic efficiency of the microorganisms is improved and the tail water treatment efficiency of domestic sewage plants is greatly improved.

Description

Magnetic sludge carbon biologic packing material of a kind of core@shell structure and its preparation method and application
Technical field
The invention belongs to technical field of sewage, more specifically, relate to magnetic sludge carbon biologic packing material of a kind of core@shell structure and its preparation method and application.
Background technology
Magnetic field can cause the series of biochemical reactions in organism, and produce biomagnetic effect, this magnetic effect can improve the biological activity of microorganism in water, accelerates biochemical reaction, thus increases its sewage treating efficiency.Such as, there are some researches show with magnetic powder to be that the microbial film of carrier is stronger than the microbial film compactness of nonmagnetic carrier, its waste water treatment efficiency improves 26%.But, magnetic exist in water not easily separated, regeneration difficulty and high in cost of production problem; And the magnetic-particle problem that then ubiquity specific surface is little or loading capacity is little, in addition, magnetic microsphere using ferrite as magnetic matrix, can lose magnetic because of the corrosive nature of microorganism or acid dissolve effect, thus limits its application in environmental area.
Typical core@shell structure material is the spheroidal particle that a class has bilayer or multilayered structure, generally by center core and be coated on outside shell and form.This nucleoid shell material not only has the function of two kinds of matrix materials, can also according to specific design, the structurizing of practical function material and functionalized, complementary specific function material of gaining the upper hand.Such as, the core stabilization of originally unstable or less stable can be made, function and characteristic that core and shell material itself do not possess can be obtained.
At present, there are no take magneticsubstance as core, mud carbon prepares correlative study and the report of the magnetic sludge carbon biologic packing material of nucleocapsid structure for shell material.
Summary of the invention
Technical problem to be solved by this invention is the technical deficiency overcoming the low and biologic packing material of existing sewage treating efficiency, provides one Fe 3o 4with mud preparation, there is the method for the mud carbon biologic packing material of core@shell structure, be specifically related to magnetize Fe 3o 4for core, with mud carbon for shell material prepares the method for core@shell structure magnetic sludge carbon biologic packing material.
The object of this invention is to provide a kind of magnetic sludge carbon biologic packing material of core@shell structure.
Another object of the present invention is to provide the preparation method of the magnetic sludge carbon biologic packing material of above-mentioned core@shell structure.
Another object of the present invention is to provide the application of the magnetic sludge carbon biologic packing material of above-mentioned core@shell structure.
Above-mentioned purpose of the present invention is achieved by the following technical programs:
A magnetic sludge carbon biologic packing material for core@shell structure is with Fe 3o 4magnetic microsphere is magnetic core, take iron containing sludge as middle layer raw material, with common sludge or zinc-containing sludge for husk as raw material, adopts dipping-furnace drying method repeatedly, middle layer raw material and husk as raw material are coated on Fe successively 3o 4on magnetic microsphere, form the precursor with core@shell structure and (be designated as Fe 3o 4@mud carbon), then obtain through 500 ~ 800 DEG C of pyrolysis and aftertreatment.
Preferably, in above-mentioned preparation technology, described Fe 3o 4magnetic microsphere is using carboxymethyl cellulose as the bonding spherical Fe of caking agent 3o 4after heat solution obtains.
Described aftertreatment refers to successively through pickling, washing and oven dry.Further, described aftertreatment is first successively after pickling, washing and oven dry, then is placed in magnetic field magnetization 30 ~ 50 min, and the magnetic Fe_3O_4@mud carbon of obtained strengthening, is the magnetic sludge carbon biologic packing material of core@shell structure.
The present invention is coated on dry Fe with iron containing sludge (iron-carbon material) 3o 4between magnetic microsphere and zinc-containing sludge, pyrolysis forms iron-carbon middle layer, as Fe 3o 4the middle layer of core and outer mud carbon, plays the effect of both links.After the magnetic sludge carbon biologic packing material of core@shell structure is successfully prepared, they is placed in upflowing bacteria bed as biologic packing material, effective advanced treatment can be carried out to the tail water of domestic sewage factory.In the process, middle iron-carbon-coating is as pure Fe 3o 4transition layer between core and shell mud carbon, plays the effect of connection.Due to Fe 3o 4@mud carbon has the different small magnetic domain in many directions, and magnetization can make the magnetic moment direction of magnetic domain in magneticsubstance become consistent, strengthens its magnetic.
In addition, as the enforceable preferred version of one, described Fe 3o 4the preparation method of magnetic microsphere is as follows: by the mass ratio of 1:1.5 ~ 2, by Fe 3o 4magnetic adds in the cmc soln of 1 ~ 2g/L, adds in spherical model the spherical Fe being squeezed into diameter 2.5 ~ 3.5mm after stirring 3o 4, these Fe 3o 4ball 80 ~ 100 DEG C of freeze-day with constant temperature 1h, then in 400 ~ 500 DEG C of heating 1h, form the Fe of diameter 1.5 ~ 2.5mm 3o 4magnetic microsphere.
Preferably, the preparation method of described iron containing sludge: by the iron mud ratio (calculating with dry mud) of 1:1, the inorganic molysite of dewatered sludge with iron content 4 mol/L is mixed, fully stirs post-drying, the iron containing sludge of obtained water ratio 90 ~ 110%.
Preferably, the preparation method of described zinc-containing sludge: by the zinc mud ratio (calculating with dry mud) of 1:1, mixes dewatered sludge with the inorganic zinc salt containing zinc 5 mol/L, and fully stirs post-drying, the zinc-containing sludge of obtained water ratio 90 ~ 110%.
More preferably, above-mentioned inorganic molysite is FeSO 4, FeCl 2or Fe (NO 3) 2; Above-mentioned inorganic zinc salt is ZnCl 2.
In addition, particularly, the preparation method of the magnetic sludge carbon biologic packing material of above-mentioned core@shell structure comprises the following steps:
S1. Fe is prepared according to the method described above 3o 4magnetic microsphere (is also designated as Fe 3o 4dry bulb);
S2. iron containing sludge and zinc-containing sludge is prepared according to the method described above;
S3. adopt dipping-furnace drying method, S2 gained iron containing sludge is coated on the Fe of S1 gained drying 3o 4on magnetic microsphere, obtained Fe 3o 4@iron containing sludge ball;
S4. adopt dipping-furnace drying method repeatedly, common sludge or S2 gained zinc-containing sludge are coated on the Fe of S3 gained drying 3o 4on@iron containing sludge ball, obtained Fe 3o 4@mud carbon ball or Fe 3o 4@iron containing sludge@zinc-containing sludge ball;
S5. by the Fe of S4 gained 3o 4@mud carbon ball or Fe 3o 4@iron containing sludge@zinc-containing sludge ball is under nitrogen 200 ml/min protects, and with the heat-up rate of 20 DEG C/min, pyrolysis 2h under 500 ~ 800 DEG C of conditions, obtained diameter is the Fe of 3.5 ~ 4.0 mm 3o 4@mud carbon, is designated as the magnetic sludge carbon of core@shell;
S6. by the Fe of S5 gained 3o 4@mud carbon, after pickling, washing and oven dry, is placed in magnetic field magnetization 30 ~ 50 min, obtained strengthening magnetic Fe 3o 4@mud carbon, i.e. the magnetic sludge carbon biologic packing material of core@shell structure.
Wherein, take zinc-containing sludge as the scheme of husk as raw material be preferred embodiment of the present invention.
In addition, preferably, Fe described in step S5 3o 4the diameter of@mud carbon is 3.6 mm.
Preferably, the magnetized time described in step S6 is 30 min.
The application in sewage and/or wastewater treatment of the magnetic sludge carbon biologic packing material of above-mentioned core@shell structure is also within protection scope of the present invention.Especially be applied to containing COD and/or N nH3sewage and/or the process of waste water.
Can embodiment as one, the mode of described application is: using the magnetic sludge carbon biologic packing material of the core@shell structure of preparation as the filler of bacteria bed, then process sewage and/or waste water.
Compared with prior art, the present invention has following beneficial effect:
The present invention take magneticsubstance as core, with mud carbon for shell material, the magnetic sludge carbon biologic packing material of obtained core@shell structure, the problem that powder magnetic material is difficult to be separated can be solved, also can because of the iris action of outer mud carbon, solving ferrite can by the problem of microbiological corrosion as magnetic matrix; Shell porous mud carbon ratio surface is large simultaneously, and carbon can be the magnetic environment that more microorganism provides growth, improves the metabolic efficiency of microorganism.
Magnetic Fe of the present invention 3o 4there is small magnetic domain at different directions in@mud carbon, magnetization can make the magnetic moment direction of magnetic domain in magneticsubstance become consistent, strengthens its magnetic, will strengthen magnetic Fe 3o 4@mud carbon is placed in upflowing bacteria bed as biologic packing material, greatly can improve the tail water processing efficiency of domestic sewage factory.
Meanwhile, the present invention using mud as raw material, the object also achieve the treatment of wastes with processes of wastes against one another, turning waste into wealth.
Embodiment
Further illustrate content of the present invention below in conjunction with specific embodiment, but should not be construed as limitation of the present invention.Without departing from the spirit and substance of the case in the present invention, the simple modification do the inventive method, step or condition or replacement, all belong to scope of the present invention.Unless stated otherwise, the present invention adopts reagent, method and apparatus are the art conventional reagent, method and apparatus.Unless stated otherwise, agents useful for same of the present invention and material are commercial.
embodiment 1Fe 3 o 4 @mud carbon (not containing zinc salt)
1, Fe 3o 4the preparation of@mud carbon (not containing zinc salt)
S1. Fe is prepared 3o 4dry bulb (Fe 3o 4magnetic microsphere): according to the mass ratio of 1:1.5 ~ 2, by Fe 3o 4magnetic adds in the cmc soln of 1 ~ 2g/L, adds in spherical model the Fe being squeezed into diameter 2.5 ~ 3.5mm after stirring 3o 4ball, in the thermostatic drying chamber of 80 ~ 100 DEG C after dry 1h, the charcoal stove of determining being placed in 400 ~ 500 DEG C heats 1h, forms Fe 3o 4dry bulb;
S2. iron containing sludge is prepared: by the iron mud ratio (calculating with dry mud) of 1:1, by dewatered sludge and the FeSO containing 4 mol/L 4solution mixes, and after fully stirring, is placed in baking oven dry, the iron containing sludge of obtained water ratio 90% ~ 110%;
S3. adopt dipping-oven drying method that the iron containing sludge of S2 is coated on the Fe of S1 3o 4on dry bulb, obtained Fe 3o 4@iron containing sludge ball;
S4. adopt repeatedly dipping-furnace drying method that the common sludge of water ratio 110% is coated on the Fe of S3 3o 4on@iron containing sludge ball, be placed in carbon-determining stove under nitrogen 200 ml/min protects, with the heat-up rate of 20 DEG C/min, pyrolysis 2 h under 500 ~ 800 DEG C of conditions, obtained particle diameter is about the Fe of 3.6 mm 3o 4@mud carbon;
S5. the Fe of core@shell structure that obtains of step S4 3o 4@mud carbon is through pickling, washing and drying and processing.
2, Fe 3o 4the performance of@mud carbon (not containing zinc salt)
(1) specific surface area is 150.6 m 2/ g, saturation magnetization is approximately 35.4 emu/g.
(2) magnetic Fe of preparation is recorded by " hole pottery acidproof, corrosion resistance nature test method (GB/T1970-1996) " 3o 4the acid resistance of@mud carbon is 91.3%.
Relatively find, acid resistance is higher by 24.1% than common magnetic sludge carbon.The Fe prepared under described common magnetic sludge carbon refers to equal conditions 3o 4equally distributed mud carbon (non-core@shell structure).
3, Fe 3o 4the application of@mud carbon (not containing zinc salt)
By the magnetic Fe of preparation 3o 4the upflowing that@mud carbon is filled in internal diameter 50 mm and the high 300 mm formation height of bed 20 mm as biologic packing material is aeration biological filter bed.When hydraulic detention time is set as 1.5 h, this bacteria bed can remove certain sanitary sewage plant tail water (COD:45.1 ppm, N stationary phase nH3: 7.2 ppm) in the COD of the 50.5% and N of 35.3% nH3.
embodiment 2Fe 3 o 4 @mud carbon (containing zinc salt)
1, Fe 3o 4the preparation of@mud carbon (containing zinc salt)
S1. Fe is prepared 3o 4dry bulb: with embodiment 1;
S2. iron containing sludge is prepared: with embodiment 1;
S3. zinc-containing sludge is prepared: by the zinc mud ratio (calculating with dry mud) of 1:1, by the ZnCl of dewatered sludge and 5 mol/L 2solution mixes, and after fully stirring, is placed in baking oven dry, the zinc-containing sludge of obtained water ratio 90% ~ 110%;
S4. adopt dipping-oven drying method that iron containing sludge is coated on Fe 3o 4obtained Fe on dry bulb 3o 4@iron containing sludge ball;
S5. adopt repeatedly dipping-furnace drying method that zinc-containing sludge is coated on above-mentioned Fe 3o 4on@iron containing sludge ball, be placed in carbon-determining stove under nitrogen 200 ml/min protects, with the heat-up rate of 20 DEG C/min, under 500 ~ 800 DEG C of conditions, pyrolysis 2 h, prepares the Fe that particle diameter is about 3.6 mm 3o 4@mud carbon;
S6. the Fe of core@shell structure that obtains of step S5 3o 4@mud carbon is through pickling, washing and drying and processing.
2, Fe 3o 4the performance of@mud carbon
(1) specific surface area is 365.6 m 2/ g, saturation magnetization is approximately 36.3 emu/g.
(2) magnetic Fe is recorded by " hole pottery acidproof, corrosion resistance nature test method (GB/T1970-1996) " 3o 4the acid resistance of@mud carbon is 90.5%.
Relatively find, higher by 24.1% than the acid resistance of common magnetic sludge carbon.The Fe prepared under described common magnetic sludge carbon refers to equal conditions 3o 4equally distributed mud carbon (non-core@shell structure).
3, Fe 3o 4the application of@mud carbon
By magnetic Fe 3o 4the upflowing that@mud carbon is filled in internal diameter 50 mm and the high 300 mm formation height of bed 20 mm as biologic packing material is aeration biological filter bed.When hydraulic detention time is set as 1.5 h, this bacteria bed can remove certain sanitary sewage plant tail water (COD:45.1 ppm, N stationary phase nH3: 7.2 ppm) in the COD of the 58.4% and N of 39.5% nH3.
Through comparative experiments display, magnetic Fe 3o 4@mud carbon ratio common sludge carbon improves 10.2% as the clearance of bacteria bed under same condition of biologic packing material.
embodiment 3 strengthens magnetic Fe 3 o 4 the preparation of@mud carbon and performance thereof
1, magnetic Fe is strengthened 3o 4the preparation of@mud carbon
S1. with embodiment 2, the Fe that particle diameter is about 3.6 mm is prepared 3o 4@mud carbon;
S2. the Fe of core@shell structure that obtains of step S1 3o 4@mud carbon is through pickling, washing, oven dry and magnetization treatment; Described magnetization magnetizes 30 min by the magnetic field of these magnetic Fe_3O_4s@mud carbon as 3000 GS, and strengthened magnetic Fe 3o 4@mud carbon.
2, magnetic Fe is strengthened 3o 4the performance of@mud carbon
(1) magnetic Fe is strengthened 3o 4the specific surface area of@mud carbon is 365.6 m 2/ g, saturation magnetization is approximately 36.3 emu/g.
(2) magnetic Fe is recorded by " hole pottery acidproof, corrosion resistance nature test method (GB/T1970-1996) " 3o 4the acid resistance of@mud carbon is 90.5%, than the magnetic sludge carbon (Fe prepared under equal conditions of non-core@shell structure 3o 4equally distributed mud carbon) acid resistance high by 24.1%.
3, magnetic Fe is strengthened 3o 4the application of@mud carbon
Magnetic Fe will be strengthened 3o 4the upflowing that@mud carbon is filled in internal diameter 50 mm and the high 300 mm formation height of bed 20 mm as biologic packing material is aeration biological filter bed.When hydraulic detention time is set as 1.5 h, this bacteria bed can remove certain sanitary sewage plant tail water (COD:45.1 ppm, N stationary phase nH3: 7.2 ppm) in the COD of the 61.5% and N of 46.6% nH3.
Through comparative experiments display, strengthening magnetic Fe 3o 4@mud carbon ratio common sludge carbon improves 19.3% as the clearance of bacteria bed under same condition of biologic packing material.

Claims (10)

1. a magnetic sludge carbon biologic packing material for core shell structure, it is characterized in that, be with Fe 3o 4magnetic microsphere is magnetic core, take iron containing sludge as middle layer raw material, with common sludge or zinc-containing sludge for husk as raw material, adopts the method for repeatedly flooding-drying, middle layer raw material and husk as raw material are coated on Fe successively 3o 4on magnetic microsphere, form the precursor with core@shell structure, then obtain through 500 ~ 800 DEG C of pyrolysis and aftertreatment.
2. the magnetic sludge carbon biologic packing material of core@shell structure according to claim 1, is characterized in that, described Fe 3o 4magnetic microsphere is using carboxymethyl cellulose as the bonding spherical Fe of caking agent 3o 4after heat solution obtains; Described aftertreatment refers to successively through pickling, washing and oven dry.
3. the magnetic sludge carbon biologic packing material of core@shell structure according to claim 1 or 2, it is characterized in that, described aftertreatment is successively after pickling, washing and oven dry, is placed in magnetic field magnetization 30 ~ 50 min.
4. the magnetic sludge carbon biologic packing material of core@shell structure according to claim 1 or 2, is characterized in that, described Fe 3o 4the preparation method of magnetic microsphere is as follows: by the mass ratio of 1:1.5 ~ 2, by Fe 3o 4magnetic adds in the cmc soln of 1 ~ 2g/L, adds in spherical model the spherical Fe being squeezed into diameter 2.5 ~ 3.5mm after stirring 3o 4, these Fe 3o 4ball 80 ~ 100 DEG C of freeze-day with constant temperature 1h, then in 400 ~ 500 DEG C of heating 1h, form the Fe of diameter 1.5 ~ 2.5mm 3o 4magnetic microsphere.
5. the magnetic sludge carbon biologic packing material of core@shell structure according to claim 1, it is characterized in that, the preparation method of described iron containing sludge: by the iron mud ratio of 1:1, the inorganic molysite of dewatered sludge with iron content 4 mol/L is mixed, abundant stirring post-drying, the iron containing sludge of obtained water ratio 90 ~ 110%;
The preparation method of described zinc-containing sludge: by the zinc mud ratio of 1:1, mixes dewatered sludge with the inorganic zinc salt containing zinc 5 mol/L, and fully stirs post-drying, the zinc-containing sludge of obtained water ratio 90 ~ 110%.
6. the magnetic sludge carbon biologic packing material of core@shell structure according to claim 5, it is characterized in that, described inorganic molysite is FeSO 4, FeCl 2or Fe (NO 3) 2; Described inorganic zinc salt is ZnCl 2.
7. the preparation method of the magnetic sludge carbon biologic packing material of the arbitrary described core@shell structure of claim 1 ~ 6, is characterized in that, comprise the following steps:
S1. Fe is prepared according to method described in claim 2 or 4 3o 4magnetic microsphere;
S2. iron containing sludge and zinc-containing sludge is prepared according to method described in claim 5;
S3. adopt dipping-furnace drying method, S2 gained iron containing sludge is coated on the Fe of S1 gained drying 3o 4on magnetic microsphere, obtained Fe 3o 4@iron containing sludge ball;
S4. adopt dipping-furnace drying method repeatedly, common sludge or S2 gained zinc-containing sludge are coated on the Fe of S3 gained drying 3o 4on@iron containing sludge ball, obtained Fe 3o 4@mud carbon ball or Fe 3o 4@iron containing sludge@zinc-containing sludge ball;
S5. by the Fe of S4 gained 3o 4@iron containing sludge ball or Fe 3o 4@iron containing sludge@zinc-containing sludge ball, under nitrogen 200 ml/min protects, with the heat-up rate of 20 DEG C/min, pyrolysis 2h under 500 ~ 800 DEG C of conditions, obtained diameter is the Fe of 3.5 ~ 4.0 mm 3o 4@mud carbon (being designated as the magnetic sludge carbon of core@shell);
S6. by the Fe of S5 gained 3o 4@mud carbon, after pickling, washing and oven dry, is placed in magnetic field magnetization 30 ~ 50 min, obtained strengthening magnetic Fe 3o 4@mud carbon, i.e. the magnetic sludge carbon biologic packing material of core@shell structure.
8. preparation method according to claim 7, is characterized in that, Fe described in step S4 3o 4the diameter of@mud carbon is 3.6 mm; The magnetized time described in step S5 is 30 min.
9. the application of magnetic sludge carbon biologic packing material in sewage and/or wastewater treatment of the arbitrary described core@shell structure of claim 1 ~ 7.
10. apply according to claim 9, it is characterized in that, described sewage and/or waste water refer to and contain by COD and/or N nH3sewage and/or waste water.
CN201510383999.7A 2015-07-03 2015-07-03 Magnetic sludge carbon biological filler with core-at-shell structure and preparation method and application thereof Expired - Fee Related CN104961228B (en)

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