CN106277173A - A kind of iron carbonyl combines superconducting magnetic and separates the method for phosphor resource in water - Google Patents

A kind of iron carbonyl combines superconducting magnetic and separates the method for phosphor resource in water Download PDF

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Publication number
CN106277173A
CN106277173A CN201610896715.9A CN201610896715A CN106277173A CN 106277173 A CN106277173 A CN 106277173A CN 201610896715 A CN201610896715 A CN 201610896715A CN 106277173 A CN106277173 A CN 106277173A
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iron carbonyl
water
adsorbent
phosphorous
superconducting magnetic
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CN201610896715.9A
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孙占学
李亦然
王学刚
周宾宾
陈程
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East China Institute of Technology
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East China Institute of Technology
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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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/16—Oxyacids of phosphorus; Salts thereof
    • C01B25/26—Phosphates
    • C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
    • 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
    • C02F1/48—Treatment of water, waste water, or sewage with magnetic or electric fields
    • C02F1/488—Treatment of water, waste water, or sewage with magnetic or electric fields for separation of magnetic materials, e.g. magnetic flocculation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2303/00—Specific treatment goals
    • C02F2303/16—Regeneration of sorbents, filters

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Analytical Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention discloses a kind of iron carbonyl and combine superconducting magnetic separation method of phosphor resource in water, it is characterised in that iron carbonyl adsorbent is added in phosphorous pending water with the dosage of 0.1 20g/l；After being sufficiently stirred for 10 30 min, the high gradient superconducting magnetic separator utilizing magnetic field intensity to be more than 3T carries out solid-liquid separation, utilize clear water or regenerate high-gradient medium containing alkali eluent, the phosphorous agitated desorbing of iron carbonyl adsorbing material after eluting and further solid-liquid separation, obtain regenerating iron carbonyl adsorbent and phosphorous alkalescence dope, hydroxy iron powder as iron carbonyl adsorbent again with, phosphorous alkalescence dope adds calcium hydroxide, calcium phosphate product prepared by calcium oxide or calcium salt.The present invention efficiently traps powder body iron carbonyl adsorbent in magnetic field, thereafter the iron carbonyl adsorbent of Phosphate Sorption is carried out alkaline hydrolysis suction, and the phosphorus dope of desorbing adds calcium salt and produces calcium phosphate, finally realizes the resource reclaim of phosphorus in water.

Description

A kind of iron carbonyl combines superconducting magnetic and separates the method for phosphor resource in water
Technical field
The invention belongs to phosphorus extractive technique field, relate to a kind of iron carbonyl and combine superconducting magnetic separation phosphor resource in water Method.
Background technology
Iron carbonyl is self-assembling formation and a class cheap ferrum system mineral that can conveniently synthesize, and common includes goethitum (Goethite, alpha-feooh), four directions goethitum (Akaganeite, β-FeOOH), lepidocrocite (Lepidocrocite, γ- FeOOH), six side's lepidocrocites (Feroxyhyte, δ-FeOOH) and ferrihydrite (Ferrihydrite, Fe5HO8·4H2O).Wherein, Bimodal ferrihydrite (2-Line Ferrihydrite) is commonly referred to as amorphous Fe oxides (Amorphous iron oxide) or hydroxyl Base ferrum oxide (Hydrous ferric oxide)
Iron carbonyl class mineral are widespread in nature, due to surface nature, micro nano structure and bigger ratio that it is active Surface area, plays a significant role in contaminant transportation conversion process.Meanwhile, numerous studies show that phosphorus is had preferably by iron carbonyl Absorbability.
It is to realize polluting the key link removed that iron carbonyl adsorbing material is separated from water, and wherein, adsorbent bed is filled and coagulation It it is the most ripe separating technology.Adsorbent bed technological requirement adsorbent has certain granularity, thus reduces the pressure of bed body Loss.The general particle diameter of iron carbonyl of self-assembling formation and commercial synthesis is relatively thin, even micro nano structure.Pelletize and load are two kinds The manufacture route of main adsorbent bed iron carbonyl base adsorbent, wherein, granular iron carbonyl (Granular ferric Hydroxide, GFH) feeding water with field of waste water treatment achieved with suitable business success, obtain wide range of industrial applications；Granule Activated carbon, haydite even load iron carbonyl also have substantial amounts of research and performance test report.
But, pelletize and load process to a certain degree have lost the good adsorbent performance of iron carbonyl micro nano structure, significantly Having raised the manufacturing cost of adsorbent, meanwhile, after adsorbent bed filling, the theoretical adsorption capacity of functional material is compared and is sufficiently mixed Adsorption process decline to a great extent.Adsorbent itself is had no special requirements by coagulation process, is widely used.Due to adsorbent with moisture During from, having swept along substantial amounts of suspended particulate substance and flocculant hydrolyzate, adsorbent cannot regeneration and mud easily be made Become secondary pollution.Therefore, there is certain defect in traditional iron carbonyl technique for applying, constrains the service efficiency of iron carbonyl, simultaneously Raise cost of water treatment.
Magneto separate is a kind of based on magnetic mineral Force principle in magnetic field, it is achieved the technology that magnetic mineral precisely separates. Magnetic field is the build-in attribute of mineral by magnetic force, its stress in magnetic fieldF mag Determined by formula (1):
(1)
In formula,For permeability of vacuum,For the volume of mineral grain,For magnetic field gradient,MFor the intensity of magnetization of mineral, It is the physical quantity relevant to magnetic field intensity, can be measured by vibration magnetic strength meter, and unit is emu/g.
According to mineral easy magnetization degree in magnetic field, mineral typically can be divided into ferromagnetism, weak magnetic and non magnetic ore deposit Thing.Strongly magnetic mineral has significant difference with the hysteresis curve of weak magnetic mineral, and strongly magnetic mineral i.e. produces bigger magnetic at downfield Square, and then by obvious magnetic force, and it i.e. can reach magnetic saturation in relatively downfield；The strongly magnetic mineral of nature is few, common Only Fe3O4、γ-Fe2O3, some ferrite, ferrum, cobalt, nickel simple substance etc..Typically there is certain table due to strongly magnetic mineral Face inertia, lacks interfacial activity group, and it is directly used in pollution adsorption treatment and has certain limitation.Meanwhile, above-mentioned strong magnetic Property mineral are the most oxidized and lose strong magnetic characteristic.
Have lot of documents at present and patent pays close attention to the surface-functionalized modification of strongly magnetic mineral, and then combine magnetic separation technique Research for pollution control.First the work of this class prepare the ferromagnetism magnetic core such as magnetic iron ore, ferrite, thereafter at magnetic Core surface covers active layer by modes such as surface deposition, functional group's graftings, and then utilizes permanent magnetism, electromagnetism or cryogenic magnetic field to carry out Separate.Such as, the patent of Application No. 201510891129.0, it, by preparing ferrite ferromagnetism magnetic core, is coated with thereafter ferrum Base gel, prepares ferromagnetism adsorbing material, utilizes cryogenic magnetic field to realize solid-liquid separation, and then processes arsenic, antimony pollution in water.This is special In profit, the main advantage utilizing superconducting magnetic separator is to compare tradition magnetic separation technique water process production capacity can be greatly improved, and raising sets Standby intensive rate.Shortcoming is, magnetic core and active layer complex process, and material preparation cost is greatly improved, and then has raised water process Cost, meanwhile, after adsorption-desorption process repeatedly, magnetic core can be broken or come off with active layer, and then causes at Magneto separate During active material significantly lose.The core concept of similar patent still utilizes strong magnetic core cladding active component to carry out pollutant Absorption, utilizes thereafter cryogenic magnetic field to separate.
Summary of the invention
The deficiency existed in view of prior art, inventor is by substantial amounts of experimental exploring, it was thus unexpectedly found that one Based on > 3T superconducting intense magnetic field and directly utilize the weak magnetic natural minerals (also can the manually low cost synthetic mineral) water as adsorbent Process technique.Iron carbonyl mineral self have strong interface activity, the most excellent environment adsorbing materials.；Meanwhile, iron carbonyl Mineral are weak-magnetism ore thing, and its stress in magnetic field increases with magnetic field intensity and improves, it is more difficult to reach magnetic saturation.But, due to ring The activity of border functional material is typically inversely proportional to particle diameter, formula (1) can obtain, and small particle mineral grain is declined to a great extent by magnetic force, passes < 1.5 T magnetic induction, the most difficult efficient trapping powder body iron carbonyl adsorbent that system magnetic separator provides.Therefore inventor Propose micron particles and cryogenic magnetic field to combine, when superconducting magnet provide more than 3T background magnetic field, can be greatly improved micro- Scale particles iron carbonyl and the separation efficiency of water, by controlling the lower limit particle size of iron carbonyl, can realize powder body iron carbonyl in work The directly application of industry water treatment field.
In sum, present invention aim at proposing a kind of new method, propose to utilize superconducting magnet to produce the strong magnetic of 3T , in conjunction with high-gradient medium, the powder body iron carbonyl being directly separated in water, it is to avoid the absorption that iron carbonyl pelletize, biofilm etc. cause The technical problem that capacity declines to a great extent and material manufacturing cost is greatly improved；Avoid the preparation of ferromagnetism magnetic core simultaneously and modification is led The adsorbing material manufacturing cost caused is substantially improved, and then provides a kind of iron carbonyl to combine superconducting magnetic separation phosphor resource in water Method, finally realize the resource reclaim of phosphorus in water.
The technical solution used in the present invention:
A kind of iron carbonyl combines superconducting magnetic and separates the method for phosphor resource in water, by iron carbonyl adsorbent with 0.1-20g/l Dosage add in phosphorous pending water；After being sufficiently stirred for 10-30 min, utilize the high gradient superconduction that magnetic field intensity is more than 3T Magnetic separator carries out solid-liquid separation, utilizes clear water or regenerates high-gradient medium containing alkali eluent, the phosphorous iron carbonyl absorption after eluting The agitated desorbing of material and further solid-liquid separation, obtain regenerating iron carbonyl adsorbent and phosphorous alkalescence dope, and hydroxy iron powder is made For iron carbonyl adsorbent again with, phosphorous alkalescence dope adds calcium hydroxide, calcium phosphate product prepared by calcium oxide or calcium salt.
Further, described iron carbonyl adsorbent is natural minerals or synthetic mineral, including goethitum, four policy ferrum Ore deposit, lepidocrocite, six side's lepidocrocite and ferrihydrites.
Further, the iron carbonyl particle size range in iron carbonyl adsorbent is 5 microns to 1000 microns；
Further, the desorbing of phosphorous iron carbonyl adsorbent uses the aqueous slkali of 0.1-2mol/l concentration.
Further, the solid-liquid separating method after the phosphorous agitated desorbing of iron carbonyl high-gradient medium after eluting uses filter pressing Or superconducting magnetic separates.
Further, magnetic induction in superconducting magnetic separator > 5T, the high-gradient medium in superconducting magnetic separator include bristle cake, Rhombus medium net, tooth plate and steel rod, trap powder body iron carbonyl adsorbent in magnetic field and carry out solid-liquid separation.
Further, the phosphorous iron carbonyl adsorbent in removal magnetic field pours alkali regenerated reactor with the concentration of 100-300g/l.
In a word, the present invention utilizes superconducting magnet to produce > 3T magnetic induction, in conjunction with bristle, rhombus medium net, tooth plate, The contour functionally gradient material (FGM) of steel rod, efficiently trapping powder body iron carbonyl adsorbent, thereafter the iron carbonyl absorption to Phosphate Sorption in magnetic field Agent carries out alkaline hydrolysis suction, and the phosphorus dope of desorbing utilizes calcium oxide precipitation to produce calcium phosphate, finally realizes the resource reclaim of phosphorus in water.
Accompanying drawing explanation
Fig. 1 is the hysteresis curve figure of the ferrihydrite of synthetic.
Fig. 2 is the process chart of embodiment 1.
Detailed description of the invention
Tie with specific embodiment that the present invention is described further below.
Embodiment 1: embodiment is an example
Shown in Fig. 1；Its synthetic method, for add in iron salt by alkali under 70rpm stirring condition, regulates pH to 6.0, static 1h, its Rear centrifugal abandoning supernatant, 60 DEG C of drying obtain the ferrihydrite powder that particle diameter is 10-100 μm.According to technological process shown in Fig. 2, Above-mentioned powder ferrihydrite adsorbent is quantitatively added in phosphorous pending water.Stir 10-30 minute, pump into thereafter superconducting magnetic separation Separating in machine, sorting chamber fills bristle medium, after sorting chamber absorption is saturated, is moved out magnetic field, utilizes and take off containing alkali cleaning Iron carbonyl is gone out sorting chamber by liquid, after agitated desorbing and further solid-liquid separation, hydroxy iron powder again with, phosphorous alkalescence is dense Liquid adds calcium oxide and prepares calcium phosphate product.
Iron carbonyl adsorbent is natural minerals or synthetic mineral, including goethitum (Goethite, alpha-feooh), and four Policy iron mine (Akaganeite, β-FeOOH), lepidocrocite (Lepidocrocite, γ-FeOOH), six side's lepidocrocites (Feroxyhyte, δ-FeOOH) and ferrihydrite (Ferrihydrite, Fe5HO8·4H2O)；
Iron carbonyl particle size range can be from 0.1 micron to 1000 micron, preferably 5 microns to 1000 microns.
Behind the removal magnetic field, high-gradient medium chamber of absorption saturated hydroxy ferrum, with clear water or alkaline eluant, hydroxy iron powder is washed De-；
The desorbing of phosphorous iron carbonyl utilizes the alkali of 0.1-2 mol/l, and alkali includes the common alkali such as sodium hydroxide, potassium hydroxide；
The separation of alkalescence phosphorus dope and iron carbonyl can also can separate with superconducting magnetic with filter pressing；
Alkalescence phosphorus dope utilizes calcium hydroxide or calcium oxide precipitation, prepares calcium phosphate, obtains product after filter pressing.
According to above process condition, municipal wastewater phosphorus concentration 5mg/l, after adding the bimodal ferrihydrite of 2g/l, phosphorus concentration Drop to 0.05mg/l.Superconducting magnet magnetic induction is effective more than 3T, and more preferably, single set superconducting magnetic separator hour processes water to 5T Measuring 500 cubes, iron carbonyl adsorbent, after the absorption of Magneto separate chamber is saturated, pours alkali regeneration with the concentration of 200g/l after exiting magnetic field Pond, the phosphorus concentration in alkali regenerated reactor can be regulated and controled by cycle-index, and alkali regenerated reactor is divided again by superconducting magnetic separation process From iron carbonyl and phosphorus dope, iron carbonyl recycles, and adds calcium oxide precipitated calcium phosphate in phosphorus dope, and residue alkali liquor reuse is to alkali Regenerated reactor.
Embodiment 2:
Utilizing the goethitum Ore naturally occurred, it is after beneficiation enrichment, and goethitum content is more than 90%, after crushing, sieving Control its particle diameter be 20 microns standby to 100 microns.Utilize above-mentioned goethitum sorbent treatment phosphate fertilizer plant sewage, phosphorus concentration 800 mg/l.Adding the goethitum (Goethite, alpha-feooh) of 10 g/l, phosphorus concentration drops to 50 mg/l.Superconducting magnet magnetic induction Intensity is more than 5T, and single set superconducting magnetic separator hour processes the water yield 300 cubes, and iron carbonyl adsorbent is saturated in the absorption of Magneto separate chamber After, pouring alkali regenerated reactor with the concentration of 200g/l after exiting magnetic field, the phosphorus concentration in alkali regenerated reactor can be carried out by cycle-index Regulation and control, alkali regenerated reactor separates iron carbonyl and phosphorus dope again by superconducting magnetic separation process, and iron carbonyl recycles, in phosphorus dope Adding calcium oxide precipitated calcium phosphate, residue alkali liquor reuse is to alkali regenerated reactor.
The foregoing is only presently preferred embodiments of the present invention, all made within the spirit and principles in the present invention appoint What amendment, equivalent and improvement etc., should be included within the scope of the present invention.

Claims (7)

1. an iron carbonyl combines superconducting magnetic and separates the method for phosphor resource in water, it is characterised in that adsorbed by iron carbonyl Agent adds in phosphorous pending water with the dosage of 0.1-20g/l；After being sufficiently stirred for 10-30 min, magnetic field intensity is utilized to be more than The high gradient superconducting magnetic separator of 3T carries out solid-liquid separation, utilizes clear water or regenerates high-gradient medium, after eluting containing alkali eluent The phosphorous agitated desorbing of iron carbonyl adsorbing material and further solid-liquid separation, obtain regenerating iron carbonyl adsorbent and phosphorous alkalescence be dense Liquid, hydroxy iron powder as iron carbonyl adsorbent again with, phosphorous alkalescence dope adds calcium hydroxide, prepared by calcium oxide or calcium salt Calcium phosphate product.
A kind of iron carbonyl the most according to claim 1 combines superconducting magnetic and separates the method for phosphor resource in water, and it is special Levying and be, described iron carbonyl adsorbent is natural minerals or synthetic mineral, including goethitum, four directions goethitum, lepidocrocite, Six side's lepidocrocite and ferrihydrites.
A kind of iron carbonyl the most according to claim 1 and 2 combines superconducting magnetic and separates the method for phosphor resource in water, its Being characterised by, the iron carbonyl particle size range in iron carbonyl adsorbent is 5 microns to 1000 microns.
A kind of iron carbonyl the most according to claim 3 combines superconducting magnetic and separates the method for phosphor resource in water, and it is special Levying and be, the desorbing of phosphorous iron carbonyl adsorbent uses the aqueous slkali of 0.1-2mol/l concentration.
A kind of iron carbonyl the most according to claim 4 combines superconducting magnetic and separates the method for phosphor resource in water, and it is special Levying and be, the solid-liquid separating method after the phosphorous agitated desorbing of iron carbonyl high-gradient medium after eluting uses filter pressing or superconducting magnetic Separate.
A kind of iron carbonyl the most according to claim 5 combines superconducting magnetic and separates the method for phosphor resource in water, and it is special Levy and be, magnetic induction in superconducting magnetic separator > 5T, the high-gradient medium in superconducting magnetic separator includes bristle cake, rhombus medium Net, tooth plate and steel rod, trap powder body iron carbonyl adsorbent in magnetic field and carry out solid-liquid separation.
A kind of iron carbonyl the most according to claim 6 combines superconducting magnetic and separates the method for phosphor resource in water, and it is special Levying and be, the phosphorous iron carbonyl adsorbent in removal magnetic field pours alkali regenerated reactor with the concentration of 100-300g/l.
CN201610896715.9A 2016-10-13 2016-10-13 A kind of iron carbonyl combines superconducting magnetic and separates the method for phosphor resource in water Pending CN106277173A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS56152790A (en) * 1980-04-25 1981-11-26 Ebara Infilco Co Ltd Treatment of waste water containing phosphorus and cod component
US5759407A (en) * 1996-02-23 1998-06-02 Gurevitz; David Method and apparatus for processing waste water
JP2005007358A (en) * 2003-06-20 2005-01-13 Japan Science & Technology Agency Magnetic separation device
CN1697784A (en) * 2003-08-07 2005-11-16 仁木工芸株式会社 Waste water treatment system by superconductive magnetic separation
CN103641214A (en) * 2013-12-10 2014-03-19 北京科技大学 Method for treating heavy metal wastewater by superconductive HGMS (high gradient magnetic separation)-FeOOH coupled technique
CN105251470A (en) * 2015-10-27 2016-01-20 四川大学 Adsorbing agent for removing phosphorus and heavy metal ions and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS56152790A (en) * 1980-04-25 1981-11-26 Ebara Infilco Co Ltd Treatment of waste water containing phosphorus and cod component
US5759407A (en) * 1996-02-23 1998-06-02 Gurevitz; David Method and apparatus for processing waste water
JP2005007358A (en) * 2003-06-20 2005-01-13 Japan Science & Technology Agency Magnetic separation device
CN1697784A (en) * 2003-08-07 2005-11-16 仁木工芸株式会社 Waste water treatment system by superconductive magnetic separation
CN103641214A (en) * 2013-12-10 2014-03-19 北京科技大学 Method for treating heavy metal wastewater by superconductive HGMS (high gradient magnetic separation)-FeOOH coupled technique
CN105251470A (en) * 2015-10-27 2016-01-20 四川大学 Adsorbing agent for removing phosphorus and heavy metal ions and preparation method thereof

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