CN106622100B - A kind of method that ferrimanganic compound combination superconduction Magneto separate arsenic removal recycles - Google Patents
A kind of method that ferrimanganic compound combination superconduction Magneto separate arsenic removal recycles Download PDFInfo
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- CN106622100B CN106622100B CN201610894493.7A CN201610894493A CN106622100B CN 106622100 B CN106622100 B CN 106622100B CN 201610894493 A CN201610894493 A CN 201610894493A CN 106622100 B CN106622100 B CN 106622100B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—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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- C—CHEMISTRY; METALLURGY
- 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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- C—CHEMISTRY; METALLURGY
- 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
- C22B7/005—Separation by a physical processing technique only, e.g. by mechanical breaking
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/103—Arsenic compounds
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a kind of methods that ferro manganese composite oxides combination superconduction Magneto separate arsenic removal recycles, it is characterized in that, the ferro manganese composite oxides are screened or cyclone classification obtains partial size greater than 10 μm or 20 μm of components are spare, and less than 10 μm or 20 μm of component backflows to preparation link crystallizes again；It is direct plungeed into or is mixed in arsenic-containing water to be processed using nature water project situation and stirred, after being sufficiently mixed reaction, obtain mixed reactant；Mixed reactant is quickly separated by solid-liquid separation using magnetic induction intensity > 3T superconducting magnetic separator；After magnetic separation quick separating, no direct qualified discharge of magnetic liquid phase has magnetic solid phase to enter in alkali activating tank；The mixed reactant of ferro manganese composite oxides and arsenic dope again passes by superconducting magnetic separator in alkali activating tank, and no magnetic liquid phase is used as arsenic dope resource utilization, and having magnetic solid phase is regenerated ferro manganese composite oxides, recycling.Its use cost is greatly reduced in the technique for greatly simplifying its industrial application.
Description
Technical field
The invention belongs to arsenic extractive technique field, it is related to what a kind of ferrimanganic compound combination superconduction Magneto separate arsenic removal recycled
Method.
Background technique
Trivalent arsenic and pentavalent arsenic are main inorganic arsenic components, and usually association exists in water body environment.Arsenic is one in water
The important environmental contaminants of kind can cause a variety of muscle, bone and the nervous system disease, more especially when containing arsenic in drinking water
Have carcinogenic, teratogenesis, mutagenic characteristic.The arsenic pollution Treatment process generally pass by educational circles and engineering circles for a long time in water
Note.
Ferrimanganic compound starts in 2005-2010 it has been reported that it is that excellent inorganic arsenic handles material, and manganese draws
Enter the treatment effect for being remarkably improved adsorbent material to trivalent arsenic, and ferriferous oxide is higher than three to the obvious processing effect of pentavalent arsenic
Valence arsenic.In water environment, trivalent arsenic and pentavalent arsenic can be converted with the Redox Condition of water body, therefore, while be gone in water removal
Trivalent arsenic and pentavalent arsenic are the key that except water process arsenic removal.
The related patents and paper of ferro manganese composite oxides are all many, concentrate on materials synthesis and go for different pollutants
Except field.For example, attempt within Zhang [1,2] etc. 2007 to be prepared for ferro manganese composite oxides, and it was prepared in 2012 mole
Than 3:1-9:1 iron: the composite material of manganese.It is separated from water however, powder adsorbent material is relatively difficult to achieve, tradition need to be granulated or combine wadding
Solidifying technique uses, and the granulation of ferrimanganic compound is abnormal difficult, and granular ferrimanganic compound is at present in engineering using few.
In the prior art, although having the application method of a small amount of work concern granular iron and manganese oxides of support type, for example, patent
200610008135.8 reporting the application method of ferro manganese composite oxides load diatomite filling adsorbent bed.But load process is not
It is evitable bring duct block and adsorption capacity decline, meanwhile, as access times increase, active component fall off seriously, into
And greatly restrict Practical Project use.At the same time, ferrimanganic compound combination flocculation process has Small Scale Industry application,
By adding powder, thereafter plus the mode of flocculant precipitating is separated from water.However, its flocculation sedimentation separation mode, due to
The cotton-shaped compound of a large amount of iron or aluminium is generated in Flocculation Settling Process, and with a large amount of suspended particulate substance is precipitated, will be led
Cause ferrimanganic compound can not circular regeneration, and cannot achieve the resource utilization of arsenic, generations sludge is hazardous waste, is greatly mentioned
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 the technology that magnetic mineral precisely separates.
It in magnetic field is the build-in attribute of mineral, the stress F in magnetic field by magnetic forcemagBy formulaIt determines:
In formula, μ0For space permeability, V is the volume of mineral grain, and gradH is magnetic field gradient, and M is that the magnetization of mineral is strong
Degree is physical quantity relevant to magnetic field strength, can pass through vibration magnetic strength meter measurement, unit emu/g.
According to easy magnetization degree of the mineral in magnetic field, mineral can be generally divided into ferromagnetism, weak magnetic and non magnetic mine
Object.The hysteresis loop of strongly magnetic mineral and weak magnetic mineral has significant difference, and strongly magnetic mineral generates 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, certain ferrites, iron, cobalt, nickel simple substance etc..Since strongly magnetic mineral generally has certain table
Face inertia lacks interfacial activity group, and being directly used in pollution adsorption treatment has certain limitation.
Although also there are related patents to pay close attention to the surface-functionalized modification of strongly magnetic mineral, and then combine magnetic separation technique for dirt
Contaminate the research administered.This kind of work usually prepare the ferromagnetisms magnetic core such as magnetic iron ore, ferrite first, 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, by preparing ferrite ferromagnetism magnetic core, being coated thereafter iron-based solidifying application No. is 201510891129.0 patent
Glue prepares ferromagnetism adsorbent material, is realized and is separated by solid-liquid separation using cryogenic magnetic field, and then handles arsenic, antimony pollution in water.But the patent
In, the main advantage using superconducting magnetic separator is can to greatly improve water process production capacity compared to traditional magnetic separation technique, improves equipment
Intensive rate.The disadvantage is that magnetic core and active layer complex process, material preparation cost greatly improve, so raised water process at
This, meanwhile, 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 substantially loses in journey.The core concept of similar patent is polluted mostly or using strong magnetic core cladding active component
Object absorption, is separated using cryogenic magnetic field thereafter.
In conclusion there is also many deficiency factors for existing arsenic removal reuse method.
Summary of the invention
In view of the shortcomings of the prior art, inventor passes through experimental exploring, it was thus unexpectedly found that one kind is based on > 3T
Superconducting intense magnetic field and directly using paramagnetism mineral as the water treatment technology of adsorbent, to reach arsenic removal recycling.Ferrimanganic is multiple
Closing oxide is paramagnetism mineral, and magnetic attribute is variant with different ferrimanganic ratios, and ferro manganese composite oxides are weak magnetic mineral,
Stress increases with magnetic field strength and is improved 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, ferrimanganic than the ferro manganese composite oxides more than or equal to 3 can > 3T superconduction it is strong
It realizes and efficiently separates in magnetic field.Powder ferro manganese composite oxides can be realized in the direct application in Treatment of Industrial Water field.
It is final real it is an object of that present invention to provide a kind of method that ferrimanganic compound combination superconduction Magneto separate arsenic removal recycles
The resource reclaim of arsenic in existing water.
The technical solution adopted by the present invention:
A kind of method that ferro manganese composite oxides combination superconduction Magneto separate arsenic removal recycles, the ferrimanganic molar ratio be greater than or
Or cyclone classification screened equal to 3 ferro manganese composite oxides obtains partial size greater than 10 μm or 20 μm of components are spare, is less than μm 10
Or 20 μm of component backflows to preparation link crystallizes again；
Powder ferro manganese composite oxides are direct plungeed into arsenic-containing water to be processed and are stirred, or are carried out using nature water project situation
Mixing, ferro manganese composite oxides are sufficiently mixed with arsenic-containing water react after, obtain mixed reactant；
Mixed reactant is quickly separated by solid-liquid separation using magnetic induction intensity > 3T superconducting magnetic separator；Superconducting magnetic separator is adopted
With reciprocating structure, sorting chamber is interior to fill high-gradient medium, 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, there are the magnetic solid phase i.e. ferro manganese composite oxides containing arsenic to wait sorting
Chamber pours in alkali activating tank after removing magnetic field；After alkali activation, ferro manganese composite oxides and arsenic dope is mixed in alkali activating tank
It closes reactant and again passes by superconducting magnetic separator, for no magnetic liquid phase as arsenic dope resource utilization, it is regenerated for having magnetic solid phase
Ferro manganese composite oxides are recycled.
Further, screening or cyclone classification process are equivalent to the sieve using 800 or 1000 mesh apertures.
Further, ferro manganese composite oxides are sufficiently mixed with arsenic-containing water reacts 10-60 minutes.
Further, the high-gradient medium in superconducting magnetic separator includes bristle cake, diamond shape medium net, tooth plate and steel rod, in magnetic
Ferro manganese composite oxides adsorbent is trapped in, and then is realized and be separated by solid-liquid separation.
Further, it removes the adsorbent of ferro manganese composite oxides containing arsenic in magnetic field and alkali regeneration is poured with the concentration of 100-300g/l
Pond.
The present invention using superconducting magnet generate > 3T magnetic induction intensity, in conjunction with bristle, diamond shape medium net, tooth plate, steel rod etc.
High gradient material, and then realize efficiently separating for ferro manganese composite oxides and water, thereafter to the ferrimanganic combined oxidation of arsenic-adsorbing
Object carries out acidolysis suction, and then realizes that sorbent circulation uses and the recycling of arsenic regenerates.It solves iron and manganese oxides and is granulated difficulty,
The technical issues of severely restricts are received in industrial application, while the technique of its industrial application is greatly simplified, and it is greatly reduced
Use cost.
Detailed description of the invention
Fig. 1 is the hysteresis loop figure of three kinds of ratio ferrimanganic compounds；
Fig. 2 is the process flow chart of embodiment 1.
Fig. 1 shows that above-mentioned three kinds of ferrimanganic compounds are soft magnetic materials, magnetic hysteresis 0, quality magnetic moment liter with magnetic field raising
Height, and magnetic saturation phenomenon is not observed in 5T.
Specific embodiment
Tie that the present invention is described further with specific embodiment below.
Embodiment 1:
With divalent iron saltAnd potassium permanganateFor raw material, guarantee that iron, manganese salt are total
Molar concentration is 2.0mol/L, prepares the ferro manganese composite oxides that Fe/Mn molar ratio is 3:1.Above-mentioned compound iron and manganese oxides are straight
1000 mesh Wet method vibration screens were connected, powder ferro manganese composite oxides are made after the washed drying of retention part；It is returned by part
It flow to material preparation link.Powder ferro manganese composite oxides are direct plungeed into arsenic-containing water to be processed, wherein predominantly trivalent arsenic,
It can use plurality of devices to be stirred, such as agitator, pipe-line mixer etc., also can use nature water project situation and mixed
It closes, such as is added in upstream, voluntarily mixed using water flow.Ferro manganese composite oxides and arsenic-containing water be sufficiently mixed 10 minutes it is i.e. reachable
To good arsenic removal efficiency, ferro manganese composite oxides and water quick separating, ferrimanganic combined oxidation can be realized using superconducting magnetic separator
Object arresting efficiency > 99%, and processing capacity is up to 500m3/ h or more.After magnetic separation, no magnetic liquid phase can direct qualified discharge, have magnetic
Solid phase enters in alkali activating tank, utilizes the arsenic of sodium hydroxide solution desorption ferrimanganic compound absorption.Ferrimanganic is compound in alkali activating tank
The mixed system of oxide and arsenic dope again passes by superconducting magnetic separator, and no magnetic liquid phase has magnetic as arsenic dope resource utilization
Solid phase is regenerated ferro manganese composite oxides, be can be recycled.
According to above process condition, river 200mg/l containing arsenic concentration, wherein major pollutants are trivalent arsenic, add 4g/
After the ferro manganese composite oxides of the ferrimanganic ratio 3:1 of l, arsenic concentration drops to 0.05mg/l.Superconducting magnet magnetic induction intensity be greater than etc.
In 3T, single to cover 300 cubes of water of superconducting magnetic separator hour processing, ferro manganese composite oxides move back after Magneto separate chamber adsorption saturation
The concentration behind magnetic field with 200g/l pours alkali desorption pool out, and the arsenic concentration in alkali desorption pool reaches 10g/l, thereafter by superconducting magnetic
Separation process separates ferrimanganic compound and arsenic dope again, and ferro manganese composite oxides recycle, and arsenic dope resourcebility utilizes.
Embodiment 2:
Rural area arsenic pollution underground water, arsenic concentration 50mg/l, wherein major pollutants are trivalent arsenic and pentavalent arsenic.With ferrous iron
SaltTrivalent iron saltAnd potassium permanganateFor raw material, guarantee that iron, manganese salt are total
Molar concentration is 3.0mol/L, prepares Fe2+/ Mn molar ratio is 3:1, Fe3+/ Mn molar ratio is 4:1, and Fe/Mn molar ratio is 7:
1 ferro manganese composite oxides.10 μm or more components are separated by cyclone classification device, washing, it is compound that drying obtains powder ferrimanganic
Oxide.After the ferro manganese composite oxides of ferrimanganic ratio 7:1 for adding 2g/l, arsenic concentration drops to 0.01mg/l.Superconducting magnet magnetic
Induction is greater than 5T, and single to cover 600 cubes of water of superconducting magnetic separator hour processing, ferro manganese composite oxides adsorbent is in Magneto separate
After chamber adsorption saturation, exits the concentration behind magnetic field with 100g/l and pour sour desorption pool, 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
It utilizes, arsenic dope can realize that resource utilization utilizes.
The foregoing is merely illustrative of the preferred embodiments of the present invention, and done within the spirit and principles of the present invention
What modifications, equivalent substitutions and improvements etc., should all be included in the protection 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 (1)
1. a kind of method that ferro manganese composite oxides combination superconduction Magneto separate arsenic removal recycles, which is characterized in that ferrimanganic molar ratio
Or cyclone classification screened more than or equal to 3 ferro manganese composite oxides obtain partial size greater than 20 μm of components it is spare, less than 20 μ
M component backflow to preparation link crystallizes again；
Powder ferro manganese composite oxides are direct plungeed into arsenic-containing water to be processed and are stirred, ferro manganese composite oxides are abundant with arsenic-containing water
After hybrid reaction 10-60 minutes, mixed reactant is obtained；
Mixed reactant is quickly separated by solid-liquid separation using magnetic induction intensity > 3T superconducting magnetic separator；Superconducting magnetic separator is using past
Duplex, the interior filling of sorting chamber include the high-gradient medium of bristle cake, diamond shape medium net, tooth plate and steel rod, are situated between to high gradient
After matter traps ferro manganese composite oxides saturation, sorting chamber removes magnetic field, and then realizes and be separated by solid-liquid separation；
Without the direct qualified discharge of magnetic liquid phase in assorting room, there is magnetic solid phase to remove the absorption of ferro manganese composite oxides containing arsenic in magnetic field
Agent is poured in alkali activating tank with the concentration of 100-300g/L；After alkali activation, ferro manganese composite oxides and arsenic in alkali activating tank
The mixed reactant of solution again passes by superconducting magnetic separator, and no magnetic liquid phase has the magnetic solid phase to be as arsenic solution resource utilization
Regenerated ferro manganese composite oxides are recycled.
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| CN108913909B (en) * | 2018-08-30 | 2024-01-30 | 西北矿冶研究院 | Black copper mud arsenic removal device and method |
| 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 |
| 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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