CN103950987A - Recycling method of pickling sludge - Google Patents
Recycling method of pickling sludge Download PDFInfo
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- CN103950987A CN103950987A CN201410146603.2A CN201410146603A CN103950987A CN 103950987 A CN103950987 A CN 103950987A CN 201410146603 A CN201410146603 A CN 201410146603A CN 103950987 A CN103950987 A CN 103950987A
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- pickling mud
- pickling
- ferrite
- recoverying
- iron
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Abstract
The invention discloses a recycling method of pickling sludge, and belongs to the solid waste material utilization technology of environmental engineering. According to the recycling method, a pickling sludge solid waste material is taken as raw material; an appropriate amount of an iron source is replenished; water is taken as a solvent; ammonium hydroxide is taken as a pH conditioning agent; a foaming agent is added; and a corresponding heavy metal hydroxide is obtained at a certain temperature under a certain pressure; the heavy metal hydroxide is taken as a precursor, and is delivered into a special physical and chemical environment which can not be realized at normal temperature under normal pressure, so that the precursor is dissolved completely, different growth units are formed, nucleation growth according to a certain combination manner is realized, stable ferrite with low leaching toxicity and high saturation magnetization degree is obtained via crystallization. The recycling method is suitable for environmental protection, and is capable of realizing recycling of pickling sludge resources, and increasing additional value of the pickling sludge resources. Particle size of the ferrite obtained via the recycling method ranges from 200 to 400nm; the ferrite is spherical particle particles, and possesses excellent crystal form and organic waste water adsorption capacity.
Description
Technical field
The solid waste the invention belongs in environmental engineering utilizes technical field, particularly a kind of recoverying and utilizing method of pickling mud.
Background technology
In steel process of manufacture, in order to improve erosion resistance and the surface quality of product, need to product, carry out surface cleaning with sulfuric acid, hydrofluoric acid and nitric acid, clean in the waste water producing and contain a large amount of spent acid.In the process that spent acid reclaims, can produce spent pickle liquor, spent pickle liquor can not directly be discharged, otherwise pollute the environment, improvement for spent pickle liquor, some iron and steel enterprises still adopt traditional treatment process, general lime, carbide slag or the calcium hydroxide of adopting carries out neutralizing treatment to it, produces a large amount of mud, i.e. pickling mud simultaneously.And the mud producing difficult treatment again, take a large amount of soils, and cause the waste of secondary pollution and resource.
According to the Hazardous Waste List > > (2008 editions) of < < country, this class pickling mud belongs to Hazardous wastes, contain a large amount of residual acid and heavy metal, especially sexavalent chrome, there is the features such as toxicity is large, easily accumulation, unstable, calorific value is low, easy loss.If do not dealt carefully with any stacking, may cause the secondary pollution of surface water, soil, underground water, even jeopardize biologic chain, cause serious harm.Yet pickling mud contains a large amount of heavy metals, as iron, chromium, nickel, zinc, etc. there is certain economic worth.Mainly take at present both at home and abroad the processing mode of landfill after solidification and stabilization.
Utilization about pickling mud, (patent publication No.: CN101037289) introduced a kind of solid waste in industrial Plate Production of utilizing that patent of invention " is recycled the method for industrial acid-washed metal sludge in Plate Production ", as mud, produce ferric oxide and black iron oxide pigment novel process for cement slurry.First metal sludge is deposited on the place in natural air and is dried, or add acid solution at metal pickling mud, make it have mobility, add again water and be warming up to more than 95 ℃, add alkaline liquid again, stir, dehydration, crushed after being dried obtain iron oxide black.Although this method makes mud can obtain part utilization, but do not consider that pickling mud itself is exactly the product after neutralization, secondary adds pickling again, and then adds alkali neutralization, quite secondary neutralization, further increased the amount of mud, also needed to heat up simultaneously, cost is high, can cause secondary pollution, also needing to consume the energy, and the difficult control of final product composition, to manufacture of cement, may impact.
Patent " discarded metal sludge recoverying and utilizing method " (patent publication No.: be CN101086035) to add in metal sludge that hydrogen peroxide and potassium permanganate carry out strong oxidation and air natural is oxidized, for the powder that iron content is high, supply with ironmaking, or production counterweight, or production raw material cement, iron level is low carries out roasting, 1200～1300 ℃ of maturing temperatures, are still after roasting with powder form and supply with ironmaking or produce counterweight.This patent is in fact still direct making cement raw material after drying sludge, cost is also will consume the resources such as hydrogen peroxide and potassium permanganate, other modes that are used with the form of powder be because can impact and be difficult to carry out ironmaking production, therefore be still a kind of low value-added method of utilizing.
Patent " a kind of recycling processing method of heavy metal sewage sludge " (patent publication No.: CN201010541598.7), it is first that 30wt%～50wt% acid solution leaches the heavy metal in sludge containing heavy metal by weight percent concentration, by frequency, be the pickling liquor of 14KHz～28KHz ultrasonication again, after ultrasonic separation 30～60min, the throw out of solid-liquid separation sulfur acid calcium and containing the acid solution of heavy metal ion, the acid solution leaching is after ferrous sulfate is processed and regulated pH value to be 9, add after ferroxidant oxidation, form ferrite.Calcium sulfate precipitation thing forms gypsum through washing with after being dried.The method complex process, and acidleach causes increasing waste liquid, the amount of additional source of iron is the ferrous sulfate of 10～20 times of weight of heavy metal weight in acidleach mixing solutions, additional too much source of iron, can cause main products in product is Z 250, and Z 250 is extremely easily oxidized to the slight weak ferric oxide of magnetic.
Summary of the invention
The object of the present invention is to provide a kind of recoverying and utilizing method of pickling mud.
The technical solution that realizes the object of the invention is:
A recoverying and utilizing method for pickling mud, described pickling mud is used for preparing ferrite, and concrete steps are as follows:
The first step, dries pickling mud, grinds, and sieves;
Second step, supplements source of iron in the first step in the pickling mud obtaining, add distilled water, and whipping agent, stirs and make former slip, adds subsequently precipitation agent to regulate behind slurry pH value to 8～13, is placed in autoclave, and carries out hydro-thermal reaction at 100 ℃～300 ℃ temperature;
The 3rd step, after reaction finishes, drives still after kettle is naturally cooled to room temperature, and the ferrite mixed solution of formation is separated through magnetic separation partition method, and washing is dried, and obtains ferrite.
Wherein, pickling mud of the present invention contains the metallic elements such as Fe, Cu, Ca, Ni, Cr, Zn, Mn, Mg conventionally, its major metal content is (wt%): Fe9.87%～50.12%, Cu0.28%～32.48%, Ca4.81%～30.12%, Ni0.02%～4.12%, Cr0.01%～4.2%, Zn0.01%～12.88%, Mn0.12%～0.84, Mg0.15～3.81%, is more than mass percent.
In the first step, pickling mud, in 105～120 ℃ of oven dry 6～12h, grinds, and crosses 100～300 mesh sieves.
In second step, described source of iron is selected iron protochloride, and the consumption quality proportioning of described pickling mud and additional source of iron is 1:1～1:5.
In second step, whipping agent is selected polyoxyethylene glycol, and whipping agent add-on counts by weight percentage, and is 5%～60% of pickling mud.
In second step, precipitation agent is selected ammoniacal liquor, and the hydro-thermal reaction time is 4～12h.
In the 3rd step, at 105～120 ℃, dry 6～12 hours.
Principle and the mechanism of the inventive method are described below:
The principle of the inventive method is typical Synthesized by Hydrothermal Method crystallite process.Conventionally using corresponding oxyhydroxide as precursor, make the specific physical chemical environment that cannot realize under a normal temperature and pressure of its experience, forerunner's physical efficiency is fully dissolved and is formed different growth units, and according to certain bind mode nucleating growth, crystallizes into stable complex ferrite.Water and whipping agent not still solvent or expanded promotor in this process, as pressure transfer medium, thereby avoided follow-up pyroprocessing by the thing chemical factor of accelerating dialysis reaction and controlling its process, and solved coprecipitation method and be agglomerated into piece problem.In pickling mud, contain a large amount of heavy metal cations, be mainly Fe
3+, Fe
2+, Ni
2+, Cr
3+, Zn
2+deng, additional suitable source of iron makes the ratio of divalent ion and trivalent ion in suitable scope, and therefore, pickling mud can go out complex ferrite by supplementing appropriate source of iron crystallization under hydrothermal condition.Pickling mud mixes with additional source of iron, distilled water, with ammoniacal liquor, regulates pH can make metallic cation in system be precipitated as metal hydroxides formation presoma, and then under hydrothermal condition, dissolve and form hydroxyl group anion title complex, as, Zn(OH)
4 2+, Fe(OH)
4-, Fe(OH)
6 3-,, Ni(OH)
4 2-, Ni(OH)
6 4-, Cr(OH)
4-deng, then interconnect according to certain mode, slough crystal water, form growth unit, then gradually grow up as crystal, finally become crystal.
Compared with prior art, its remarkable advantage is in the present invention: (1), by pickling mud and additional source of iron hydrothermal ferrite, is fully used pickling mud, realizes the object of resource recycling; Not only can obtain generation complex ferrite, and can alleviate environmental pollution, be conducive to environment protection.(2) the prepared ferrite particle diameter of the present invention is little, general 200～400 nanometers, granularity all with, do not need high-temperature calcination aftertreatment.The crystal forming is comparatively complete, and purity is high, and has higher activity.(3) ferrite that prepared by the present invention is the tropeolin-D in adsorbable organic waste water also, has good treatment effect, and adsorptive capacity is large, and this ferrite sorbent material of percent of decolourization has stronger magnetic, recyclable regeneration recycling, and cost is low, environmental protection and energy saving, easy handling.
Accompanying drawing explanation
Fig. 1 is the XRD figure of pickling mud in the present invention.
Fig. 2 is the ferritic XRD figure of products therefrom of the present invention.
Fig. 3 is the ferritic SEM figure of products therefrom of the present invention.
Fig. 4 is the ferritic VSM figure of products therefrom of the present invention.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
One, a kind of recoverying and utilizing method of pickling mud
Embodiment 1
Process and the step of the present embodiment are as described below:
Heavy Metals content (wt%) in pickling mud is shown in following table 1:
Table 1 pickling main heavy metals in sludge content (wt%)
| Element | Fe | Cu | Ni | Cr | Zn | Mn | Mg | Cd | Pb | Ag | Ca |
| G/100g dewatered sludge | 40.32 | 2.00 | 0.52 | 0.62 | 0.42 | 0.43 | 1.4 | UD | UD | UD | 12.93 |
Pickling mud, in 105 ℃ of oven dry 12h, is ground, cross 100 mesh sieves;
Take 1g pickling mud and 1g iron protochloride is put into Erlenmeyer flask, add 20ml distilled water to form slurries;
Add 0.05g polyoxyethylene glycol again, stir and make former slip, add subsequently ammoniacal liquor to regulate after slurry pH value to 11, be placed in autoclave, and carry out hydro-thermal reaction at 200 ℃ of temperature, the reaction times is 8h; After after completion of the reaction kettle being naturally cooled to room temperature, drive still;
The ferrite mixed solution forming is separated through magnetic separation partition method, then uses after deionized water wash 6～8 times, dries 12 hours at 105 ℃, obtains ferrite.
The XRD figure spectrum of ortho acid contaminate mud is shown in Fig. 1, and the ferritic XRD figure of products therefrom of the present invention is shown in Fig. 2, and as can be seen from Figure 1, former electroplating sludge is without obvious diffraction peak, in amorphous state.And by after hydrothermal treatment consists, the ferrite obtaining, is to be mainly magnesium iron ferrite, and crystallization is better, can see the diffraction peak of several complex ferrites in Fig. 2.
The ferritic SEM figure of products therefrom of the present invention is shown in Fig. 3, and the result of SEM shows that the particle diameter of the complex ferrite of gained of the present invention is: 200～400 nanometers are spherical particle, with chain form, mutually combine.
The ferritic VSM figure of products therefrom of the present invention is shown in Fig. 4, and VSM result shows that the saturation magnetization of the complex ferrite product of gained of the present invention is 116.83emu/g.
By BET-N2 surface analysis method, measure ferrite specific surface area, its specific surface area is 28.67m
2/ g.
Embodiment 2
Heavy Metals content (wt%) in pickling mud is shown in following table 2:
Table 2 pickling main heavy metals in sludge content (wt%)
| Element | Fe | Cu | Ni | Cr | Zn | Mn | Mg | Cd | Pb | Ag | Ca |
| G/100g dewatered sludge | 50.12 | UD | 0.14 | 0.58 | 0.18 | 0.12 | 1.6 | UD | UD | UD | 6.14 |
Pickling mud, in 110 ℃ of oven dry 10h, is ground, cross 200 mesh sieves;
Take 1g pickling mud and 2g iron protochloride is put into Erlenmeyer flask, add 30ml distilled water to form slurries; Add 0.35g polyoxyethylene glycol again, stir and make former slip, add subsequently ammoniacal liquor to regulate after slurry pH value to 7, be placed in autoclave, and carry out hydro-thermal reaction at 300 ℃ of temperature, the reaction times is 4h;
After after completion of the reaction kettle being naturally cooled to room temperature, drive still; The ferrite mixed solution forming is separated through magnetic separation partition method, then uses after deionized water wash 6～8 times, dries 10 hours at 115 ℃, obtains ferrite.
Embodiment 3
Heavy Metals content (wt%) in pickling mud is shown in following table 3:
Table 3 pickling main heavy metals in sludge content (wt%)
| Element | Fe | Cu | Ni | Cr | Zn | Mn | Mg | Cd | Pb | Ag | Ca |
| G/100g dewatered sludge | 18.27 | 3.00 | 0.17 | 0.27 | 1.15 | 0.12 | 1.65 | 0.12 | UD | UD | 12.93 |
Pickling mud, in 120 ℃ of oven dry 6h, is ground, cross 300 mesh sieves;
Take 1g pickling mud 5g iron protochloride and put into Erlenmeyer flask, add 40ml distilled water to form slurries; Add 0.5g polyoxyethylene glycol again, stir and make former slip, add subsequently ammoniacal liquor to regulate after slurry pH value to 13, be placed in autoclave, and carry out hydro-thermal reaction at 100 ℃ of temperature, the reaction times is 12h;
After after completion of the reaction kettle being naturally cooled to room temperature, drive still; The ferrite mixed solution forming is separated through magnetic separation partition method, then uses after deionized water wash 6～8 times, dries 10 hours at 115 ℃, obtains ferrite.
Two, in the present embodiment 1, the ferritic solid Leaching of Hydrothermal Synthesis is analyzed as follows:
After ferrite Hydrothermal Synthesis, adopt U.S.'s solid waste toxicity leaching method (TCLP) to analyze solid Leaching.
Leaching agent A: measure the Glacial acetic acid of 5.7mL, add in 500mL distilled water, then add the NaOH64.3mL of 1mol/L, arrive 1L, this pH value of solution=4.93 ± 0.05 with distilled water diluting.
Leaching agent B: measure the Glacial acetic acid of 5.7mL, add in 500mL distilled water, arrive 1L, this pH value of solution=2.88 ± 0.05 with distilled water diluting.
Using pH=2.88 ± 0.05 and the HAC-NaAC buffer agent solution of PH=4.93 ± 0.05 as digestion agent, solid-to-liquid ratio is: 1:20, the rotating speed roller vibration 18h of 30 ± 2rpm/min, after standing 0.5h, with millipore filtration suction filtration, filtrate is placed in sealing and closes Plastic Bottle and test its heavy metal concentration.
Pickling mud supplements after source of iron hydrothermal treatment consists, HAC-NaAC buffer agent solution analysis heavy metal Leaching with pH=4.93 ± 0.05, be starkly lower than U.S. TCLP(Toxic Charateristic Leaching Procedure) and the toxicity judging standard value of GB (GB5085.3-2007), as Table 2,3.As can be seen here, pickling mud has the features such as stable lattice, compact structure after hydrothermal treatment consists, can reach the standard of solidification and stabilization.
Before and after table 4 hydrothermal ferriteization, Leaching changes (pH=4.93 ± 0.05)
Table 5 leaching characteristic identification standard
Note: "-" represents that legal system does not limit
Three, the tropeolin-D of the ferrite application of the present embodiment 1 preparation in absorption organic waste water, process is as follows:
Get the simulated wastewater that 30mL tropeolin-D content is 50mg/L, put into Erlenmeyer flask, the ferrite sorbent material that adds 10mg to prepare, regulate wastewater pH=7,150 ℃ of vibration absorption of oil heating in water bath, adsorption time is 5h, mixed solution is measured tropeolin-D concentration in filtrate after 0.22 μ m membrane filtration.Discovery decolorizing efficiency is high, and adsorption efficiency reaches 80.23%, calculates loading capacity and reaches 120.34mg/g.
Reaction finishes only to need with the ferrite in magnet separation solution, can obtain the liquid to be measured of clarification, without centrifugal process.
During methyl orange balance, with absolute ethanol washing, reclaiming ferrite sorbent material is for absorption for the second time, loading capacity is 119.45mg/g, reclaiming ferrite sorbent material is for absorption for the third time, and loading capacity is 117.32mg/g, as can be seen here, after reusing three times, loading capacity does not have obviously and reduces, and ferrite prepared by the present invention can reuse absorption methyl orange solution.
Claims (7)
1. a recoverying and utilizing method for pickling mud, is characterized in that, described pickling mud is used for preparing ferrite, and concrete steps are as follows:
The first step, dries pickling mud, grinds, and sieves;
Second step, supplements source of iron in the first step in the pickling mud obtaining, add distilled water, and whipping agent, stirs and make former slip, adds subsequently precipitation agent to regulate behind slurry pH value to 8～13, is placed in autoclave, and carries out hydro-thermal reaction at 100 ℃～300 ℃ temperature;
The 3rd step, after reaction finishes, drives still after kettle is naturally cooled to room temperature, and the ferrite mixed solution of formation is separated through magnetic separation partition method, and washing is dried, and obtains ferrite.
2. the recoverying and utilizing method of pickling mud according to claim 1, is characterized in that, in the first step, in described pickling mud, major metal content is (wt%): Fe9.87%～50.12%, Cu0.28%～32.48%, Ca4.81%～30.12%, Ni0.02%～4.12%, Cr0.01%～4.2%, Zn0.01%～12.88%, Mn0.12%～0.84, Mg0.15～3.81%, Cl2.34%～5.92%, S0.32%～12.23%, impurity 10%～20%; Below be all weight percentage.
3. the recoverying and utilizing method of pickling mud according to claim 1, is characterized in that, in the first step, pickling mud, in 105～120 ℃ of oven dry 6～12h, grinds, and crosses 100～300 mesh sieves.
4. the recoverying and utilizing method of pickling mud according to claim 1, is characterized in that, in second step, described source of iron is selected iron protochloride, and the consumption quality proportioning of described pickling mud and additional source of iron is 1:1～1:5.
5. the recoverying and utilizing method of pickling mud according to claim 1, is characterized in that, in second step, whipping agent is selected polyoxyethylene glycol, and whipping agent add-on counts by weight percentage, and is 5%～60% of pickling mud.
6. the recoverying and utilizing method of pickling mud according to claim 1, is characterized in that, in second step, precipitation agent is selected ammoniacal liquor, and the hydro-thermal reaction time is 4～12h.
7. the recoverying and utilizing method of pickling mud according to claim 1, is characterized in that, in the 3rd step, dries 6～12 hours at 105～120 ℃.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104437502A (en) * | 2014-12-15 | 2015-03-25 | 南京理工大学 | Magnetic fenton catalyst spinel ferrite employing fenton iron sludge as iron source and application of magnetic fenton catalyst spinel ferrite |
| CN107673409A (en) * | 2017-11-21 | 2018-02-09 | 环境保护部南京环境科学研究所 | The system and method for MgZn ferrite is prepared using pickling sludge and pickle liquor |
| CN108190886A (en) * | 2018-02-13 | 2018-06-22 | 张慕风 | For the mixing sludge adsorbing material of dye wastewater treatment |
| CN109133549A (en) * | 2018-09-04 | 2019-01-04 | 许晓原 | The processing method of acid washing phosphorization sludge |
| CN110404543A (en) * | 2019-07-12 | 2019-11-05 | 上海大学 | The VOC catalyst and preparation method thereof that metal composite oxide and ferroso-ferric oxide ordered arrangement are characterized |
| CN111233043A (en) * | 2020-01-14 | 2020-06-05 | 刘文治 | Method for preparing heavy metal-containing ferrite by resource treatment of heavy metal sludge, ferrite and application |
| CN111662571A (en) * | 2017-12-12 | 2020-09-15 | 佛山市大千色釉料有限公司 | Preparation method of ceramic pigment |
| TWI737298B (en) * | 2020-05-13 | 2021-08-21 | 崑山科技大學 | Method of rapid treatment of heavy metal sludge and preparation of ferrite magnets |
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| CN101092250A (en) * | 2006-06-20 | 2007-12-26 | 中国科学院兰州化学物理研究所 | Method for preparing magnetic Nano material |
| CN101565304A (en) * | 2009-04-30 | 2009-10-28 | 上海大学 | Method for treating electroplating sludge and pickle liquor cooperative with hydrothermal ferrite |
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| CN101092250A (en) * | 2006-06-20 | 2007-12-26 | 中国科学院兰州化学物理研究所 | Method for preparing magnetic Nano material |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104437502A (en) * | 2014-12-15 | 2015-03-25 | 南京理工大学 | Magnetic fenton catalyst spinel ferrite employing fenton iron sludge as iron source and application of magnetic fenton catalyst spinel ferrite |
| CN104437502B (en) * | 2014-12-15 | 2017-01-04 | 南京理工大学 | Magnetic fenton catalyst ferrospinel with Fenton iron containing sludge as source of iron and application |
| CN107673409A (en) * | 2017-11-21 | 2018-02-09 | 环境保护部南京环境科学研究所 | The system and method for MgZn ferrite is prepared using pickling sludge and pickle liquor |
| CN111662571A (en) * | 2017-12-12 | 2020-09-15 | 佛山市大千色釉料有限公司 | Preparation method of ceramic pigment |
| CN111662571B (en) * | 2017-12-12 | 2021-09-03 | 佛山市大千色釉料有限公司 | Preparation method of ceramic pigment |
| CN108190886A (en) * | 2018-02-13 | 2018-06-22 | 张慕风 | For the mixing sludge adsorbing material of dye wastewater treatment |
| CN109133549A (en) * | 2018-09-04 | 2019-01-04 | 许晓原 | The processing method of acid washing phosphorization sludge |
| CN110404543A (en) * | 2019-07-12 | 2019-11-05 | 上海大学 | The VOC catalyst and preparation method thereof that metal composite oxide and ferroso-ferric oxide ordered arrangement are characterized |
| CN110404543B (en) * | 2019-07-12 | 2022-06-14 | 上海大学 | VOC catalyst with characteristic of ordered arrangement of composite metal oxide and ferroferric oxide and preparation method thereof |
| CN111233043A (en) * | 2020-01-14 | 2020-06-05 | 刘文治 | Method for preparing heavy metal-containing ferrite by resource treatment of heavy metal sludge, ferrite and application |
| TWI737298B (en) * | 2020-05-13 | 2021-08-21 | 崑山科技大學 | Method of rapid treatment of heavy metal sludge and preparation of ferrite magnets |
| US11524904B2 (en) | 2020-05-13 | 2022-12-13 | Kun Shan University | Method of rapid treatment of heavy metal sludge and preparation of ferrite magnets |
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Application publication date: 20140730 |