CN106315740B - A method of utilizing high-iron fly ash dephosphorization - Google Patents
A method of utilizing high-iron fly ash dephosphorization Download PDFInfo
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- CN106315740B CN106315740B CN201610900335.8A CN201610900335A CN106315740B CN 106315740 B CN106315740 B CN 106315740B CN 201610900335 A CN201610900335 A CN 201610900335A CN 106315740 B CN106315740 B CN 106315740B
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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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
- C02F1/488—Treatment of water, waste water, or sewage with magnetic or electric fields for separation of magnetic materials, e.g. magnetic flocculation
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Abstract
The invention discloses a kind of methods using high-iron fly ash dephosphorization, belong to resources circulation and environment protection field, it is characterized by: high-iron fly ash to be obtained to the high-speed rail microparticle of partial size≤10 μm, Iron grade >=52% through ball milling, magnetic separation and screening process, and its surface is cleaned by ultrasonic by weak acid；The pH value of phosphorus-containing wastewater is adjusted to 3-5；High-speed rail microparticle is added in phosphorus-containing wastewater, lasting stirring is lower to contain phosphonium ion in absorption effluent；Under neutral or weak basic condition, make to be desorbed containing phosphonium ion from high-speed rail microparticle surfaces, then can be separately recovered through Magneto separate and utilize high-speed rail microparticle and solution containing phosphate.It is not only fast and effective, environmentally protective that the method for the present invention handles phosphorus-containing wastewater, and the high-speed rail microparticle after can be used repeatedly.
Description
Technical field
It is specifically a kind of by adjusting pH value, utilizing high-speed rail the present invention relates to a kind of processing method of phosphorus-containing wastewater
The method that fly ash grain realizes phosphorous ionic adsorption.
Background technique
Water eutrophication is one of the protrusion environmental threat that China faces, and effectively controls water eutrophication and gives birth to holding
State balance, effective use water resource are most important.The essence of water eutrophication is algae largely numerous life, and algae is to the need of nutrition
Seeking ratio is C: H: O: N: P=106: 263: 110: 16: 1, it is seen that phosphorus is the Optimal Control factor for administering water eutrophication.Cause
This, realizes that economic, efficient dephosphorization becomes the key for administering water eutrophication.
Absorption method is the most popular method of low concentration solute phosphorus in removal, mainly the physics of solid absorbent is utilized to inhale
Chemisorption performance is echoed, the phosphorus in waste water is removed.In common phosphorus adsorbent, flyash as a kind of trade waste,
Have many advantages, such as from a wealth of sources, cheap, specific surface area is larger, and applying in phosphorus adsorbing domain has larger potentiality.Publication number
Show for the patent of invention of CN105293614A using flyash as adsorbent for phosphate removal, under conditions of adjusting pH value of waste water,
50% or more is reached to total dephosphorization efficiency of the phosphorus-containing wastewater of middle and high concentration.After Phosphate Sorption, adsorbent needs are separated with water body, but
Fine particles when due to adsorbent application, thus separation of solid and liquid is complicated and difficult, or even causes secondary pollution, significantly limits
The industrial application of coal ash phosphorus sorbent.
Magneto separate is a kind of solid-liquid separation technique of strength, if introducing phosphorus sewage treatment, can greatly improve solid-liquid point
From efficiency.It, can be from by magnetic separation comprising a part with magnetic microballon, i.e. high-iron fly ash or Fly ash bead in flyash
It separates and obtains in flyash.If doing phosphorus adsorbent using high-iron fly ash, after completing phosphorus absorption, adsorbent can utilize Magneto separate
Technology realizes high efficient solid and liquid separation.In existing paper document, Wang Longgui, in December, 2003, Chinese Mining Industry utilizes high-iron fly ash
Removal of Phosphorus in Wastewater is matched with high-gradient magnetic field, phosphorus ligands amount is 0.6mg/g.Wang Jinshan etc., in March, 2008, flyash, hair
When high-iron fly ash now is used alone as phosphorus adsorbent, dephosphorization amount is only 0.55mg/g；And by high-iron fly ash and aluminum sulfate
When flocculant is used in combination, best dephosphorization amount is up to 4.55mg/g.Phosphorus in Domestic Wastewater with Pulverized content is about 8-15mg/L, industrial phosphorus-containing
Sewage phosphorus content is higher, and up to thousands of mg/L, and the discharge standard of China's phosphorus-containing wastewater is 1 grade of discharge 0.5mg/L, 2 grades of discharges
For 1mg/L.Although as it can be seen that can realize quick separation of solid and liquid, high-speed rail under magnetic field using high-iron fly ash processing phosphorus-containing wastewater
The phosphorus adsorbance of flyash itself is too low；High-iron fly ash partial size is larger (40-50 μm of average grain diameter) simultaneously, and density is again very big
(3.2-3.6kg/m3), suspension in water is poor, thus is not able to satisfy the demand of industrial wastewater dephosphorization.
Summary of the invention
The present invention is provided a kind of using high-speed rail to avoid the deficiency that above-mentioned existing method phosphorus adsorbance is low, suspension is poor
The method of flyash dephosphorization, it is intended to first by the way that high-iron fly ash is carried out ball milling and magnetic separation again, to reduce its partial size, increase it
Iron grade；Then by adjusting phosphorus-containing wastewater pH value, make the zeta current potential positive value of high-iron fly ash, to realize that efficient phosphorus is inhaled
It is attached.
Containing phosphonium ion usually with PO4 3-、HPO4 2-And H2PO4 -Etc. forms be present in water body, it is negatively charged, therefore be easy to
Electrostatic attraction occurs with the positively charged adsorbent in surface to remove from sewage to be adsorbed by rapid physical.Hair of the invention
Bright people it has been investigated that, high-iron fly ash (be less than zero-potential point, such as pH < 5) under certain acid condition has positive table
Face zeta current potential, the wherein better effect of the ferromagnetism high-iron fly ash lotus positive electricity of Iron grade >=52%.Therefore when pH value is less than
When the zero-potential point of high-iron fly ash, high-iron fly ash can to containing phosphonium ion carry out rapid physical absorption, through Magneto separate, it can be achieved that
Efficient dephosphorization.
The method that the present invention utilizes high-iron fly ash dephosphorization, ball milling and selected, pH value including magnetic bead are adjusted, phosphorus adsorbs,
The recycling each unit process of high-speed rail microparticle, specific as follows:
Step 1, the selected of high-iron fly ash, ball milling and pretreatment
Flyash is passed through into multiple magnetic separation, ball milling and screening, obtains partial size≤10 μm, high-speed rail micro- of Iron grade >=52%
Grain, specific method is: flyash being crossed 200 meshes first, is scanned under high-intensity magnetic field to flyash using magnetic separator, is obtained
High-iron fly ash；Grinding is carried out to high-iron fly ash using ball mill or other disintegrating apparatus, is then carried out again in low-intensity magnetic field
Magnetic separation obtains the micro- magnetic bead of ferromagnetism, and the particle of partial size > 10 μm is removed using cyclone or screening plant.Gained high-speed rail micro-
Grain partial size≤10 μm, Iron grade >=52%, specific saturation magnetization >=20emu/g, average grain diameter≤5 μm.The magnetic separation includes
All kinds of magnetic selection methods such as dry method, wet process, high gradient；The ball milling should guarantee magnetic bead in ball milling mistake by modes such as logical protective gas
It is not oxidized in journey.
High-speed rail microparticle is placed in the diluted acid of 0.1mol/L and is ultrasonically treated 1-3 minutes, after Magneto separate, 110 DEG C of dryings are prevented
Tide saves backup.
Step 2, pH value are adjusted
According to the difference of high-speed rail microparticle surfaces property, the pH value of phosphorus-containing wastewater is adjusted between 3-5 using diluted acid
A certain numerical value, to guarantee high-speed rail microparticle surfaces zeta current potential >=+5mV.
Step 3, phosphorus absorption
With vigorous stirring with the additive amount of 0.2-3.0g/L to phosphorus-containing wastewater be added high-speed rail microparticle, with 200-600 turn/
The revolving speed divided persistently stirs 60-120 minutes, that is, reaches the saturation absorption of phosphor in sewage.
The recycling of step 4, high-speed rail microparticle
The high-speed rail microparticle of Phosphate Sorption is separated with water body using magnetic field；Then in the high-speed rail microparticle of Phosphate Sorption being placed in
Property or alkalescent water in, stir 2 minutes, make phosphonium ion from high-speed rail microparticle surfaces be desorbed；High-speed rail micro- is recycled by Magneto separate
Grain, then reused after diluted acid is ultrasonically treated.
The present invention detects the pattern of high-iron fly ash and high-speed rail microparticle by scanning electron microscope and laser particle analyzer
And change of size, utilize the zeta current potential of zeta potentiometer detection high-speed rail microparticle.Phosphorus content using preparation is 20mg/L's
Phosphorus-containing wastewater carries out phosphorus adsorption experiment, and the concentration of phosphorus is then determined with the absorption standard curve of phosphorus.The standard curve of phosphorus passes through molybdenum
The anti-spectrophotometry measurement of antimony.
Compared with the prior art, the beneficial effects of the present invention are embodied in:
1, simple process, at low cost, is easy to industrial application: the method for the present invention does not include complicated chemical process, except a small amount of
Diluted acid outside be without the use of chemicals；And the acid that pH is consumed required for adjusting is seldom, one cubic metre of pH value of sewage water is adjusted to 5 from 7,
Only need the hydrochloric acid of 0.01mol.The method of the present invention is more greatly simplified compared to link than traditional phosphorus adsorption method, relevant water process is set
It applies and is also greatly decreased, dephosphorization cost can be substantially reduced, convenient for industrial application.
2, strong applicability, phosphorus adsorption rate are fast: the various Phos and majority that the method for the present invention is suitable for adsorbing in waste water have
Machine phosphorus, and 60-120 minutes are close to adsorption saturation, are saturated phosphorus adsorbance up to 10.44mg/g, compared with high-iron fly ash
Adsorption capacity improves 98.7%.
3, be easy to be separated by solid-liquid separation: the method for the present invention using ball milling it is selected after high-iron fly ash as phosphorus adsorbent, have
Compared with ferromagnetism, thus adsorbent is made to be easy to solve non magnetic adsorbent by magnetic plant Magneto separate and be not easy to separate with water body
Problem.
4, the method for the present invention belongs to waste recycling using high-iron fly ash as phosphorus adsorbent, low in cost；And it used
High-speed rail microparticle can be also recycled for multiple times by recycling process, therefore have significant economic benefit and Environmental Effect
Benefit.
Detailed description of the invention
Fig. 1 is the size distribution curve of high-iron fly ash and high iron powder microparticle that laser particle analyzer detects.By scheming
Know about 41.09 μm of average grain diameter of high-iron fly ash；And about 4.37 μm of the average grain diameter of high-speed rail microparticle, all grain diameters
Respectively less than 10 μm.
Fig. 2 is the zeta current potential of high-speed rail microparticle with the change curve of pH value, therefrom it can be found that the zero of high-iron fly ash
Potential point (pH value when i.e. surface zeta potential current potential is zero) is pH=5.21, i.e., as the pH of water body < 5.21, high-speed rail microparticle tool
There is positive zeta current potential；Known in figure as pH=4, the zeta current potential of high-speed rail microparticle is+5.16mV.
Fig. 3 is at 25 DEG C, adds 1.5g/L high-speed rail microparticle in the phosphorus-containing wastewater that phosphorus content is 20mg/L, with 600 turns/
Divide electric stirring 10 minutes, is then persistently stirred 110 minutes with 300 revs/min, the change curve of phosphorus adsorption rate and time.By scheming
It is found that high-speed rail microparticle is most fast in the absorption of preceding 10 minutes phosphorus, it is then gradually slack-off；About adsorbed at 75 minutes close to saturation phosphorus,
Saturated extent of adsorption is 10.03mg/g.
Specific embodiment
The invention will be described in further detail with reference to the accompanying drawings and embodiments.
Embodiment 1:
1, the selected of high-iron fly ash, ball milling and pretreatment:
Flyash is crossed into 200 meshes first, magnetic separation then is carried out to flyash using magnetic separator, obtains high-speed rail fine coal
Ash, Iron grade are about 42%.Ball milling is carried out to high-iron fly ash under conditions of inflated with nitrogen, is then removed using dense medium cyclone
The particle of partial size > 10 μm finally carries out magnetic separation in low-intensity magnetic field again, obtains final high-iron fly ash, as shown in Figure 1,
Its Iron grade about 55.8%, average grain diameter be 4.37 μm, specific saturation magnetization 27.3emu/g.
It is ultrasonically treated 2 minutes in the dilute hydrochloric acid for the 0.1mol/L that 10g high-speed rail microparticle is placed in 200mL, utilizes neodymium iron boron
Permanent magnet assists Magneto separate, is then dried in vacuo at 110 DEG C, is finally placed in drying basin and saves backup.
2, phosphorus-containing wastewater is prepared:
Utilize KH2PO4Prepare the simulation phosphorus-containing wastewater that phosphorus content is 20mg/L；And experiment phosphorus-containing wastewater is only good the day makes
With.
3, pH value is adjusted:
As shown in Fig. 2, the zero-potential point of high-speed rail microparticle is 5.21, but away from the closer pH model of zero-potential point through detecting
In enclosing, the positive zeta potential value of high-speed rail microparticle band is lower.It, will for 0.1mol/L dilute hydrochloric acid using concentration to guarantee flocculating effect
The pH value of phosphorus-containing wastewater is adjusted to 4, and the zeta current potential of high-speed rail microparticle is+5.16mV at this time.
4, high-speed rail microparticle Removal of Phosphorus in Wastewater is utilized:
With vigorous stirring, high-speed rail microparticle, 600 revs/min of electric mixings are added in phosphorus-containing wastewater with the ratio of 1.5g/L
It mixes 10 minutes, is then persistently stirred 110 minutes with 300 revs/min, every 10-30 minutes extraction 1mL solution, pass through purple after dilution
Outside-visible absorption spectra detects its absorbance, then compares with phosphorus standard absorption curve, the residual concentration of phosphorus is determined, such as Fig. 3 institute
Show.Through examining, under 25 DEG C of room temperature, the maximum phosphorus adsorbance of high-speed rail microparticle is up to 10.44mg/g, with former high-iron fly ash phase
98.7% is improved than adsorption capacity.For the phosphorus-containing wastewater of various concentration, the phosphorus adsorbance of high-speed rail microparticle at identical temperature
Variation is little；But as the temperature increases, the phosphorus adsorbance of high-speed rail microparticle is promoted, and reaches the time of saturation absorption
It reduces.
5, the separation of solid and liquid of high-speed rail microparticle with recycle:
High-speed rail microparticle is inhaled in container bottom using neodymium iron boron strong magnet, water is outwelled, that is, realizes and is separated by solid-liquid separation.It will inhale
The high-speed rail microparticle of attached phosphorus is placed in 20mL water, adjusts pH value to 7, NaOH lye is added dropwise if necessary.Utilize Nd-Fe-B permanent magnetic
Magneto separate obtains high-speed rail microparticle to iron again, and remaining is high-density phosphorus solution.High-speed rail microparticle is again through 0.1mol/L's
Dilute hydrochloric acid ultrasonic cleaning, drying can be reused for phosphorus absorption；After 3 reuses, the high-iron fly ash rate of recovery is 78.4%.
Claims (2)
1. a kind of method using high-iron fly ash dephosphorization, it is characterised in that:
Step 1, the selected of high-iron fly ash, ball milling and pretreatment
Flyash is passed through into multiple magnetic separation, ball milling and screening, obtains partial size≤10 μm, Iron grade >=52%, stronger than saturated magnetization
Degree >=20emu/g, average grain diameter≤5 μm high-speed rail microparticle；
High-speed rail microparticle is placed in the diluted acid of 0.1mol/L and is ultrasonically treated 1-3 minutes, after Magneto separate, 110 DEG C of dryings, moisture-proof guarantor
It deposits spare；
Step 2, pH value are adjusted
According to the difference of high-speed rail microparticle surfaces property, the pH value of phosphorus-containing wastewater is adjusted to 3-5 using diluted acid, to guarantee high-speed rail
Microparticle surfaces zeta current potential >=+5mV；
Step 3, phosphorus absorption
High-speed rail microparticle, additive amount 0.2-3.0g/L, with 200-600 revs/min is added to phosphorus-containing wastewater with vigorous stirring
Revolving speed persistently stirs 60-120 minutes, that is, reaches the saturation absorption of phosphor in sewage；
The recycling of step 4, high-speed rail microparticle
The high-speed rail microparticle of Phosphate Sorption is separated with water body using magnetic field；Then by the high-speed rail microparticle of Phosphate Sorption be placed in it is neutral or
It in alkalescent water, stirs 2 minutes, phosphonium ion is desorbed from high-speed rail microparticle surfaces；High-speed rail microparticle is recycled by Magneto separate, then
It is reused after diluted acid is ultrasonically treated.
2. according to the method described in claim 1, it is characterized by: the diluted acid is hydrochloric acid, sulfuric acid or acetic acid.
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| CN108579670B (en) * | 2018-05-04 | 2021-03-30 | 南京信息工程大学 | Method for removing phosphorus by using argil |
| US10882022B2 (en) | 2018-08-07 | 2021-01-05 | King Abdulaziz University | Method of removing organic pollutants from water using ball milled and sonicated oil fly ash powder |
| CN112620117A (en) * | 2019-09-24 | 2021-04-09 | 中国科学院过程工程研究所 | Method for separating heavy metal elements from fly ash |
| CN114276815B (en) * | 2020-09-27 | 2022-11-29 | 中国科学院过程工程研究所 | Preparation method of modified fly ash, modified fly ash prepared by preparation method and application of modified fly ash |
| CN116474713A (en) * | 2023-05-04 | 2023-07-25 | 中建生态环境集团有限公司 | Efficient magnetic nano adsorption material and preparation method and application thereof |
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