CN106622100A - Method for removing arsenic for recycling by aid of ferro-manganese compound in combination with superconducting magnetic separation - Google Patents
Method for removing arsenic for recycling by aid of ferro-manganese compound in combination with superconducting magnetic separation Download PDFInfo
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- CN106622100A CN106622100A CN201610894493.7A CN201610894493A CN106622100A CN 106622100 A CN106622100 A CN 106622100A CN 201610894493 A CN201610894493 A CN 201610894493A CN 106622100 A CN106622100 A CN 106622100A
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- 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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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- 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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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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
- C02F1/48—Treatment of water, waste water, or sewage with magnetic or electric fields
- C02F1/481—Treatment of water, waste water, or sewage with magnetic or electric fields using permanent magnets
- C02F1/482—Treatment of water, waste water, or sewage with magnetic or electric fields using permanent magnets located on the outer wall of the treatment device, i.e. not in contact with the liquid to be treated, e.g. detachable
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/04—Obtaining arsenic
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/103—Arsenic compounds
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Abstract
The invention discloses a method for removing arsenic for recycling by aid of a ferro-manganese compound in combination with superconducting magnetic separation. The method is characterized in that a ferro-manganese composite oxide is screened or subjected to cyclone classification, components with the particle size larger than 10 mu m or 20 mu m are obtained for standby use, and components with the particle size smaller than 10 mu m or 20 mu m are returned to a preparation procedure for recrystallization; the ferro-manganese composite oxide is directly put into to-be-treated arsenic-containing water or mixed with the to-be-treated arsenic-containing water under a natural water conservancy condition sufficiently and reacts, and a mixture reactant is obtained; the mixture reactant is subjected to rapid solid-liquid separation by means of a superconducting magnetic separator with the magnetic induction intensity higher than 3T; after rapid magnetic separation, a non-magnetic liquid phase is directly discharged after meeting the standard, and a magnetic solid phase enters an alkali activation pool; the mixture reactant of the ferro-manganese composite oxide and concentrated arsenic liquor in the alkali activation pool enters the superconducting magnetic separator, a non-magnetic liquid phase is taken as the concentrated arsenic liquor for resource utilization, and a magnetic solid phase is the recycled ferro-manganese composite oxide and can be recycled. The industrial application process is greatly simplified, and the use cost is substantially reduced.
Description
Technical field
The invention belongs to arsenic extractive technique field, is related to what a kind of ferrimanganic compound was recycled with reference to the arsenic removal of superconduction Magneto separate
Method.
Background technology
Trivalent arsenic and pentavalent arsenic are main inorganic arsenic components, and usually association is present in water body environment.Arsenic is one in water
Important environmental contaminants are planted, especially when when containing arsenic in drinking water, various muscle, bone and the nervous system disease can be caused, more
Have carcinogenic, teratogenesis, mutagenic characteristic.Arsenic pollution Treatment process is subject to for a long time the generally pass of educational circles and engineering circles in water
Note.
Ferrimanganic compound begins with document report in 2005-2010, it is that excellent inorganic arsenic processes material, and manganese draws
Enter to be remarkably improved sorbing material to arsenious treatment effect, and ferriferous oxide is higher than three to the obvious processing effect of pentavalent arsenic
Valency arsenic.In water environment, trivalent arsenic can be converted with pentavalent arsenic with the Redox Condition of water body, therefore, while going in eliminating water
Trivalent arsenic and pentavalent arsenic are the keys except water process arsenic removal.
The Patents and paper of ferro manganese composite oxides are all many, concentrate on materials synthesis and go for different pollutants
Except field.For example, Zhang [1,2] etc. 2007 attempts being prepared for ferro manganese composite oxides, and is prepared in 2012 mole
Than 3:1-9:1 iron:The composite of manganese.However, powder sorbing material is relatively difficult to achieve being separated from water, tradition need to granulate or combine wadding
Solidifying technique is used, and the granulation of ferrimanganic compound is abnormal difficult, and granular ferrimanganic compound is at present using few in engineering.
In prior art, although have the application process of the granular iron and manganese oxides of a small amount of work concern support type, for example, patent
200610008135.8 report the using method that ferro manganese composite oxides load diatomite fills adsorbent bed.But load process is not
It is evitable to bring duct to block and adsorption capacity decline, meanwhile, as access times increase, active component comes off seriously, enters
And greatly constrain Practical Project and use.At the same time, ferrimanganic compound combines the existing Small Scale Industry application of flocculation process,
By adding powder, the mode that flocculant precipitation is added thereafter is separated from water.However, the detached mode of its flocculation sediment, due to
The cotton-shaped compound of a large amount of iron or aluminium is produced in Flocculation Settling Process, and with the substantial amounts of suspended particulate substance of precipitation, will be led
Cause ferrimanganic compound cannot circular regeneration, and cannot realize that the resource of arsenic is reclaimed, generations sludge is hazardous waste, is greatly carried
High cost of water treatment, and then greatly constrain the industrial applications of ferro manganese composite oxides.
Magneto separate is a kind of based on magnetic mineral Force principle in magnetic field, realizes magnetic mineral precisely detached technology.
It is the build-in attribute of mineral by magnetic force in magnetic field, its stress F in magnetic fieldmagBy formulaDetermine：
In formula, μ0For space permeability, V is the volume of mineral grain, and gradH is magnetic field gradient, and M is strong for the magnetization of mineral
Degree, it is the physical quantity related to magnetic field intensity, can be determined by vibration magnetic strength meter, and unit is emu/g.
Mineral can be typically divided into ferromagnetism, weak magnetic and non magnetic ore deposit by the easy magnetization degree according to mineral in magnetic field
Thing.Strongly magnetic mineral has significant difference with the hysteresis curve of weak magnetic mineral, and strongly magnetic mineral produces larger magnetic in downfield
Square, and then by obvious magnetic force, and it can reach magnetic saturation in compared with downfield；The strongly magnetic mineral of nature is few, common
Only Fe3O4、γ-Fe2O3, some ferrites, iron, cobalt, nickel simple substance etc..Because strongly magnetic mineral typically has certain table
Face inertia, lacks interfacial activity group, and it is directly used in pollution adsorption treatment and has certain limitation.
Although also there is Patents concern strongly magnetic mineral surface-functionalized modified, and then it is used for dirt with reference to magnetic separation technique
The research that dye is administered.The work of this class generally prepares first the ferromagnetism magnetic core such as magnetic iron ore, ferrite, thereafter on magnetic core surface
Active layer is covered by modes such as surface deposition, functional group's graftings, and then is separated using permanent magnetism, electromagnetism or cryogenic magnetic field.
For example, the patent of Application No. 201510891129.0, it coats iron-based and coagulates by preparing ferrite ferromagnetism magnetic core, thereafter
Glue, prepares ferromagnetism sorbing material, and using cryogenic magnetic field separation of solid and liquid is realized, and then processes arsenic, antimony pollution in water.But the patent
In, it is to compare traditional magnetic separation technique to greatly improve water process production capacity using the main advantage of superconducting magnetic separator, improve equipment
Intensive rate.Have the disadvantage, magnetic core and active layer complex process, material preparation cost is greatly improved, so raised water process into
This, meanwhile, Jing after adsorption-desorption process repeatedly, magnetic core can be broken or come off with active layer, and then cause in Magneto separate mistake
Active material significantly loses in journey.The core concept of similar patent is polluted mostly or using strong magnetic core cladding active component
Thing adsorbs, and is separated using cryogenic magnetic field thereafter.
In sum, also there is many deficiency factors in existing arsenic removal reuse method.
The content of the invention
In view of the deficiency that prior art is present, inventor passes through experimental exploring, it was thus unexpectedly found that one kind is based on>3T
Superconducting intense magnetic field and directly by the use of paramagnetism mineral as the water treatment technology of adsorbent, to reach arsenic removal recycling.Ferrimanganic is answered
It is paramagnetism mineral to close oxide, and its magnetic attribute is variant with different ferrimanganic ratios, and ferro manganese composite oxides are weak magnetic mineral, its
Stress increases with magnetic field intensity and improves in magnetic field, it is more difficult to reach magnetic saturation, applicant have further found that, by controlling ferrimanganic
The lower limit particle size of composite oxides is 10 or 20 μm, and ferro manganese composite oxides of the ferrimanganic ratio more than or equal to 3 can be>The superconduction of 3T is strong
Realize efficiently separating in magnetic field.It is capable of achieving direct application of the powder ferro manganese composite oxides in Treatment of Industrial Water field.
Present invention aim at a kind of method that ferrimanganic compound is recycled with reference to the arsenic removal of superconduction Magneto separate is provided, it is final real
The resource reclaim of arsenic in existing water.
The technical solution used in the present invention：
A kind of ferro manganese composite oxides combine the arsenic removal of superconduction Magneto separate recycle method, the ferrimanganic mol ratio be more than or
Ferro manganese composite oxides equal to 3 are screened or cyclone classification obtains particle diameter more than 10 μm or 20 μm of components are standby, less than μm 10
Or 20 μm of component backflows are crystallized again to link is prepared；
Powder ferro manganese composite oxides are direct plungeed in pending arsenic-containing water and is stirred, or carried out using nature water project situation
Mixing, ferro manganese composite oxides are sufficiently mixed after reaction with arsenic-containing water, obtain mixed reactant；
Using magnetic induction intensity>3T superconducting magnetic separators carry out quick separation of solid and liquid to mixed reactant；Superconducting magnetic separator is adopted
With filling high-gradient medium in reciprocating structure, sorting chamber, after high-gradient medium trapping ferro manganese composite oxides saturation, sorting
Chamber removes magnetic field；
In assorting room without magnetic liquid phase can direct qualified discharge, have the magnetic solid phase i.e. ferro manganese composite oxides containing arsenic to wait to sort
Chamber removes to be poured in alkali activating tank behind magnetic field；After alkali activation, ferro manganese composite oxides are mixed with arsenic dope in alkali activating tank
Close reactant and again pass by superconducting magnetic separator, without magnetic liquid phase as arsenic dope recycling, there is what magnetic solid phase had as regenerated
Ferro manganese composite oxides, recycle.
Further, screening or cyclone classification process are equivalent to the screen cloth using 800 or 1000 mesh apertures.
Further, ferro manganese composite oxides are sufficiently mixed reaction 10-60 minutes with arsenic-containing water.
Further, the high-gradient medium in superconducting magnetic separator includes bristle cake, rhombus medium net, tooth plate and steel rod, in magnetic
Ferro manganese composite oxides adsorbent is trapped in, and then realizes separation of solid and liquid.
Further, the adsorbent of ferro manganese composite oxides containing arsenic for removing magnetic field pours alkali regeneration with the concentration of 100-300g/l
Pond.
The present invention is produced using superconducting magnet>3T magnetic induction intensity, with reference to bristle, rhombus medium net, tooth plate, steel rod etc.
High gradient material, and then efficiently separating for ferro manganese composite oxides and water is realized, thereafter to the ferrimanganic combined oxidation of arsenic-adsorbing
Thing carries out acidolysis suction, and then realizes that sorbent circulation is regenerated using the resource with arsenic.Solve iron and manganese oxides granulation difficult,
The technical problem of severely restricts is received in commercial Application, while greatly simplifying the technique of its commercial Application, and it is greatly reduced
Use cost.
Description of the drawings
Fig. 1 is the hysteresis curve figure of three kinds of ratio ferrimanganic compounds；
Fig. 2 is the process chart of embodiment 1.
Fig. 1 shows that above-mentioned three kinds of ferrimanganic compounds are soft magnetic materials, and magnetic hysteresis is 0, and its quality magnetic moment is raised with magnetic field and risen
Height, and magnetic saturation phenomenon is not observed in 5T.
Specific embodiment
Tie with specific embodiment that the present invention is described further below.
Embodiment 1：
With divalent iron saltAnd potassium permanganateFor raw material, it is ensured that iron, manganese salt are total
Molar concentration is 2.0mol/L, and it is 3 to prepare Fe/Mn mol ratios:1 ferro manganese composite oxides.Above-mentioned compound iron and manganese oxides are straight
1000 mesh Wet method vibration screens were connected, after the scrubbed drying in retention part powder ferro manganese composite oxides were made；Returned by part
It flow to material and prepares link.Powder ferro manganese composite oxides are direct plungeed in pending arsenic-containing water, wherein predominantly trivalent arsenic,
Can be stirred using plurality of devices, for example agitator, pipe-line mixer etc., it is also possible to mixed using nature water project situation
Close, for example, add in upstream, voluntarily mixed using current.Ferro manganese composite oxides and arsenic-containing water be sufficiently mixed 10 minutes it is i.e. reachable
To good arsenic removal efficiency, using superconducting magnetic separator ferro manganese composite oxides and water quick separating, ferrimanganic combined oxidation are capable of achieving
Thing arresting efficiency>99%, and disposal ability is up to 500m3/ more than h.After magnetic separation, without magnetic liquid phase can direct qualified discharge, have magnetic
Solid phase is entered in alkali activating tank, and using sodium hydroxide solution the arsenic of ferrimanganic compound absorption is desorbed.Ferrimanganic is combined in alkali activating tank
Oxide again passes by superconducting magnetic separator with the mixed system of arsenic dope, without magnetic liquid phase as arsenic dope recycling, there is magnetic
The ferro manganese composite oxides that solid phase has as regenerated, can be recycled.
According to above process condition, river course 200mg/l containing arsenic concentration, wherein major pollutants are trivalent arsenic, add 4g/
The ferrimanganic of l compares 3:After 1 ferro manganese composite oxides, arsenic concentration drops to 0.05mg/l.Superconducting magnet magnetic induction intensity more than etc.
In 3T, single set superconducting magnetic separator hour processes 300 cubes of the water yield, and ferro manganese composite oxides are moved back after the adsorption saturation of Magneto separate chamber
Go out behind magnetic field and alkali desorption pool is poured with the concentration of 200g/l, the arsenic concentration in alkali desorption pool reaches 10g/l, thereafter by superconducting magnetic
Separation process separates again ferrimanganic compound and arsenic dope, and ferro manganese composite oxides are recycled, and arsenic dope resourcebility is utilized.
Embodiment 2：
Rural area arsenic pollution underground water, wherein arsenic concentration 50mg/l, major pollutants are trivalent arsenic and pentavalent arsenic.With ferrous iron
SaltTrivalent iron saltAnd potassium permanganateFor raw material, it is ensured that iron, manganese salt are total
Molar concentration is 3.0mol/L, prepares Fe2+/ Mn mol ratios are 3:1, Fe3+/ Mn mol ratios are 4:1, and Fe/Mn mol ratios are 7:
1 ferro manganese composite oxides.More than 10 μm components, washing are separated by cyclone classification device, drying obtains powder ferrimanganic and is combined
Oxide.The ferrimanganic for adding 2g/l compares 7:After 1 ferro manganese composite oxides, arsenic concentration drops to 0.01mg/l.Superconducting magnet magnetic
Induction is more than 5T, and single set superconducting magnetic separator hour processes 600 cubes of the water yield, and ferro manganese composite oxides adsorbent is in Magneto separate
After the adsorption saturation of chamber, exit behind magnetic field and sour desorption pool is poured with the concentration of 100g/l, the arsenic concentration in sour desorption pool reaches 2g/l
More than, ferro manganese composite oxides and arsenic dope, ferro manganese composite oxides circulation are separated again thereafter by superconducting magnetic separation process
Utilize, arsenic dope is capable of achieving resource and recycles.
The foregoing is only presently preferred embodiments of the present invention, it is all made within the spirit and principles in the present invention appoint
What modification, equivalent and improvement etc., should be included within the scope of the present invention.
[1]G.Zhang,J.Qu,H.Liu,R.Liu,R.Wu,Preparation and evaluation of a
novel Fe-Mn binary oxide adsorbent for effective arsenite removal,Water
Research,41(2007)1921–1928.
[2]G.Zhang,H.Liu,J.Qu,W.Jefferson,Arsenate uptake and arsenite
simultaneous sorption and oxidation by Fe-Mn binary oxides:influence of Mn/Fe
ratio,pH,Ca2+,and humic acid,Journal of Colloid and Interface Science,366
(2012)141–146.
Claims (5)
1. a kind of ferro manganese composite oxides combine the method that the arsenic removal of superconduction Magneto separate is recycled, it is characterised in that the ferrimanganic rubs
You obtain particle diameter more than 10 μm by or cyclone classification more screened than the ferro manganese composite oxides more than or equal to 3 or 20 μm of components are standby
With less than 10 μm or 20 μm of component backflows are crystallized again to links are prepared；
Powder ferro manganese composite oxides are direct plungeed in pending arsenic-containing water and is stirred, or mixed using nature water project situation
Close, ferro manganese composite oxides are sufficiently mixed after reaction with arsenic-containing water, obtain mixed reactant；
Using magnetic induction intensity>3T superconducting magnetic separators carry out quick separation of solid and liquid to mixed reactant；Superconducting magnetic separator is using past
Filling high-gradient medium in duplex, sorting chamber, after high-gradient medium trapping ferro manganese composite oxides saturation, sorting chamber is moved
Go out magnetic field；
In assorting room without magnetic liquid phase can direct qualified discharge, have the magnetic solid phase i.e. ferro manganese composite oxides containing arsenic to treat that sorting chamber is moved
In going out behind magnetic field to pour alkali activating tank；After alkali activation, ferro manganese composite oxides are anti-with the mixing of arsenic dope in alkali activating tank
Answer thing to again pass by superconducting magnetic separator, without magnetic liquid phase as arsenic dope recycling, there is the ferrimanganic that magnetic solid phase has as regenerated
Composite oxides, recycle.
2. a kind of ferrimanganic compound according to claim 1 combines the method that the arsenic removal of superconduction Magneto separate is recycled, its feature
It is that screening or cyclone classification process are equivalent to the screen cloth using 800-1000 mesh aperture.
3. a kind of ferrimanganic compound according to claim 1 combines the method that the arsenic removal of superconduction Magneto separate is recycled, its feature
It is that ferro manganese composite oxides are sufficiently mixed reaction 10-60 minutes with arsenic-containing water.
4. a kind of ferrimanganic compound according to claim 1 combines the method that the arsenic removal of superconduction Magneto separate is recycled, its feature
It is that the high-gradient medium in superconducting magnetic separator includes bristle cake, rhombus medium net, tooth plate and steel rod, and iron is trapped in magnetic field
Manganese composite oxide adsorbent, and then realize separation of solid and liquid.
5. a kind of ferrimanganic compound according to claim 1 combines the method that the arsenic removal of superconduction Magneto separate is recycled, its feature
It is that the adsorbent of ferro manganese composite oxides containing arsenic for removing magnetic field pours alkali regenerated reactor with the concentration of 100-300g/l.
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| CN109529758A (en) * | 2018-12-13 | 2019-03-29 | 东华理工大学 | Mg-Fe double-metal hydroxide adsorbent, preparation method and application |
| CN111003776A (en) * | 2019-12-30 | 2020-04-14 | 昆明理工大学 | Method for treating nonferrous smelting arsenic-containing wastewater by using ferromanganese ore |
| CN112028189A (en) * | 2020-08-24 | 2020-12-04 | 中国电建集团港航建设有限公司 | Environment-friendly superconducting magnetic separation equipment for treating domestic sewage |
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| CN111003776A (en) * | 2019-12-30 | 2020-04-14 | 昆明理工大学 | Method for treating nonferrous smelting arsenic-containing wastewater by using ferromanganese ore |
| CN112028189A (en) * | 2020-08-24 | 2020-12-04 | 中国电建集团港航建设有限公司 | Environment-friendly superconducting magnetic separation equipment for treating domestic sewage |
| CN112028189B (en) * | 2020-08-24 | 2022-08-09 | 中国电建集团港航建设有限公司 | Environment-friendly superconducting magnetic separation equipment for treating domestic sewage |
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