CN102815762A - Method for absorbing precipitation by nano iron and removing phosphate in water by magnetic separation technology - Google Patents
Method for absorbing precipitation by nano iron and removing phosphate in water by magnetic separation technology Download PDFInfo
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- CN102815762A CN102815762A CN2012103147009A CN201210314700A CN102815762A CN 102815762 A CN102815762 A CN 102815762A CN 2012103147009 A CN2012103147009 A CN 2012103147009A CN 201210314700 A CN201210314700 A CN 201210314700A CN 102815762 A CN102815762 A CN 102815762A
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Abstract
The invention discloses a method for absorbing precipitation by nano iron and removing phosphate in water by the magnetic separation technology. The method includes the following steps of firstly, extracting anhydrous ethanol to a three-neck flask, dropwise adding NaBH4 solution to FeSO4 solution to react to obtain nano-iron suspension under protection of argon; secondly, adding the nano-iron suspension to phosphate solution, regulating pH, performing oscillatory reaction in a constant-temperature oscillation box under anaerobic condition, and allowing for standing above a magnet; and thirdly, performing solid-liquid separation, extracting supernatant, and removing phosphate in water. Phosphate in water is removed by absorbing effect of nano iron and effect of generating chemical precipitation of Fe2+ and PO43- by anaerobic corrosion of nano iron, magnetism of nano iron is utilized to perform quick solid-liquid separation, and accordingly pollution remediation is achieved. The method is simple to implement, excellent in effect and free of secondary pollution and has broad application prospect in sewage treatment.
Description
Technical field
The present invention relates to a kind of adsorption precipitation of nanometer iron and magnetic separation technique of utilizing and remove phosphatic method in the water, belong to water treatment field.
Background technology
Along with the mankind increase environmental resources development and use active day by day; The agricultural run-off that is rich in sewage, the trade effluent of nitrogen, phosphorus in a large number and contains agricultural chemicals, chemical fertilizer enters in the water bodys such as lake, river; Increased the load of water nutrition material; To such an extent as to the body eutrophication pollution incident frequently takes place, and big quantity research has confirmed that phosphorus is the key constraints that makes body eutrophication.Therefore, the content of effectively removing phosphorus in the draining has become the main path that prevents body eutrophication, also is an important topic of sewage treatment area.At present, sewage dephosphorization method commonly used has biological process and chemical method.The biological phosphate-eliminating process is complicated, and wherein influenced by extraneous factors such as temperature, pH value and dissolved oxygen bigger for polyP bacteria, and the water outlet effect is difficult for stable.Though chemical dephosphorization is higher to the clearance of phosphorus, it is high to remove cost, and the use of a large amount of dephosphorization agents can cause the huge and not tractable consequence of sludge quantity, and the calcium phosphate precipitation and the water sepn that generate need long time.
Increasing in recent years research and utilization nanometer iron specific surface area characteristics big, that reactive behavior is high are carried out WWT, study its treatment effect apparently higher than micron-sized Zero-valent Iron.The adsorptive power that nanometer iron is stronger can be adsorbed the phosphate anion in the sewage fast and effectively, and the Fe of its corrosion formation
2+Meeting and phosphate radical form deposition, to strengthen phosphor-removing effect.
On the other hand, because the mutual magneticaction of nano iron particles, the zeroth order nano iron particles can be assembled very soon, in view of this, the invention provides the isolating technological method of dephosphorization of a kind of nanometer iron and magnetic and removes the phosphoric acid salt in the sewage.The present invention utilizes the magnetic of himself to make solid-liquid separation, has shortened disengaging time greatly.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, provide a kind of adsorption precipitation of nanometer iron and magnetic separation technique of utilizing to remove phosphatic method in the water.This nanometer Tie Tong crosses absorption and removes the phosphoric acid salt in the water body with chemical precipitation, and utilizes the magnetic of nanometer iron to make solid-liquid separation, repairs the purpose of polluting thereby reach.
The present invention realizes through following technical scheme:
Utilize adsorption precipitation of nanometer iron and magnetic separation technique to remove that phosphatic method may further comprise the steps in the water:
1) getting absolute ethyl alcohol 100ml in the 500ml there-necked flask, behind the logical argon gas 20min, is the NaBH of 0.4mol/L with 200mL concentration under argon shield
4It is 0.2mol/L FeSO that solution dropwise joins 200ml concentration
4Reaction obtains the nanometer iron suspension-s that concentration is 4.48g/L in the solution;
2) be to add nanometer iron suspension-s in the aqueous phosphate solution of 5 ~ 20mg/L to concentration; The concentration that makes nanometer iron is 0.1 ~ 0.6g/L; Regulate the pH value to 4-8 through dripping hydrochloric acid or sodium hydroxide solution; Under anaerobic in rotating speed is the constant-temperature shaking case of 200 rpm, carry out oscillatory reaction 1-3 h, be statically placed in magnet top 2-3min;
3) solid-liquid separation is taken out supernatant, realizes phosphatic removal in the water body.
Step 2) in, described anaerobic condition is through airtight realization after the argon gas deoxygenation.Step 2) in, said magnet is diameter 30mm, the disk of thick 10mm, all nanometer iron in the ability absorption reaction.
The beneficial effect that the present invention compared with prior art has is:
1. because nanometer abrasive grit footpath is little, specific surface area is big, has very strong adsorptive power, can effectively remove the phosphoric acid salt in the water body, and boundless application prospect is arranged in WWT.
2. the anaerobism corrosion in water of nanometer iron can produce ferrous ion, can further improve phosphatic clearance through chemical precipitation, makes water quality reaching standard.
3. the present invention utilizes the magnetic of nanometer body, has realized the sharp separation of solid-liquid in the water body, the removal of experimental pollution thing.
4. nanometer iron is cheap, just can remove phosphoric acid salt in the water fast at normal temperatures and pressures, and equipment is simple, and is easy to operate, and can not cause secondary pollution.
Description of drawings
Fig. 1 (a) is the transmission electron microscope picture of the nanometer iron that the present invention adopted;
Fig. 1 (b) is the sem photograph of the nanometer iron that the present invention adopted;
Fig. 2 for nanometer iron under the condition of different pH of the present invention to phosphatic removal effect figure.
Embodiment
Nanometer iron used in the present invention is synthetic by the laboratory, and being prepared in the there-necked flask of nanometer iron carried out, and gets absolute ethyl alcohol 100ml in the 500ml there-necked flask, behind the logical argon gas 20min, under argon shield, is the NaBH of 0.4mol/L with 200mL concentration
4It is 0.2mol/L FeSO that solution dropwise joins 200ml concentration
4In the solution, the ultimate density of obtained nanometer iron is 4.48g/L.Its transmission electron microscope is as shown in Figure 1, and visible nano iron particles is spherical in shape, particle diameter 30 ~ 80nm.Fig. 2 is the sem photograph of new preparation nanometer iron, and nano iron particles is chain and reunites, and this is because magnetic nano-particle receives coefficient results such as magnetostatic power and the surface tension between telluric magnetic force, small-particle.
Experiment is carried out in the 250ml serum bottle, the finite concentration aqueous phosphate solution is reached the nanometer iron that newly prepares add, and is diluted to 200ml with the anaerobic deionized water, seals after the argon gas deoxygenation, places the constant-temperature shaking case.Behind reaction 1 ~ 3h; After serum bottle is statically placed in magnet top 2 ~ 3min; The throw out that the overwhelming majority has been adsorbed phosphatic nanometer iron and iron rapid enrichment under the effect of magnetic force is taken out the water sample after supernatant is processing to the side near magnet, measures its phosphatic concentration.
Embodiment 1:
1) getting absolute ethyl alcohol 100ml in the 500ml there-necked flask, behind the logical argon gas 20min, is the NaBH of 0.4mol/L with 200mL concentration under argon shield
4It is 0.2mol/L FeSO that solution dropwise joins 200ml concentration
4Reaction obtains the nanometer iron suspension-s that concentration is 4.48g/L in the solution;
2) be to add nanometer iron suspension-s in the aqueous phosphate solution of 5mg/L to concentration; The concentration that makes nanometer iron is 0.1g/L; Regulate pH value to 4 through dripping hydrochloric acid solution, under anaerobic in rotating speed is the constant-temperature shaking case of 200 rpm, carry out oscillatory reaction 1 h, be statically placed in 2min above the magnet;
3) solid-liquid separation is taken out supernatant, realizes phosphatic removal in the water body, through measuring phosphate concn in the supernatant, calculates clearance.After testing, the concentration of nanometer iron is 0.1 g/L, and initial phosphate concn is 5mg/L, is 55.69% to phosphatic clearance behind the reaction 1h.
Embodiment 2:
1) getting absolute ethyl alcohol 100ml in the 500ml there-necked flask, behind the logical argon gas 20min, is the NaBH of 0.4mol/L with 200mL concentration under argon shield
4It is 0.2mol/L FeSO that solution dropwise joins 200ml concentration
4Reaction obtains the nanometer iron suspension-s that concentration is 4.48g/L in the solution;
2) be to add nanometer iron suspension-s in the aqueous phosphate solution of 20mg/L to concentration; The concentration that makes nanometer iron is 0.6g/L; Regulate pH value to 8 through dropping sodium solution; Under anaerobic in rotating speed is the constant-temperature shaking case of 200 rpm, carry out oscillatory reaction 3 h, be statically placed in magnet top 3min;
3) solid-liquid separation is taken out supernatant, realizes phosphatic removal in the water body, through measuring phosphate concn in the supernatant, calculates clearance.After testing, the concentration of nanometer iron is 0.6 g/L, and initial phosphate concn is 12mg/L, is 72.12% to phosphatic clearance behind the reaction 3h.
Embodiment 3:
1) getting absolute ethyl alcohol 100ml in the 500ml there-necked flask, behind the logical argon gas 20min, is the NaBH of 0.4mol/L with 200mL concentration under argon shield
4It is 0.2mol/L FeSO that solution dropwise joins 200ml concentration
4Reaction obtains the nanometer iron suspension-s that concentration is 4.48g/L g/L in the solution;
2) be to add nanometer iron suspension-s in the aqueous phosphate solution of 10mg/L to concentration; The concentration that makes nanometer iron is 0.4g/L; Regulate pH value to 6 through dripping hydrochloric acid solution, under anaerobic in rotating speed is the constant-temperature shaking case of 200 rpm, carry out oscillatory reaction 2 h, be statically placed in 2min above the magnet;
3) solid-liquid separation is taken out supernatant, realizes phosphatic removal in the water body, through measuring phosphate concn in the supernatant, calculates clearance.After testing, the concentration of nanometer iron is 0.4 g/L, and initial phosphate concn is 10mg/L, is 78.89% to phosphatic clearance behind the reaction 2h.
Embodiment 4: implementation step is identical with embodiment 3, is to add nanometer iron suspension-s in the aqueous phosphate solution of 10mg/L to concentration, makes the concentration of nanometer iron be respectively 0.1; 0.2,0.4,0.6g/L; Behind the 2h phosphatic clearance is reached 34.49,38.68,78.89 and 87.01% respectively.
Embodiment 5: implementation step is identical with embodiment 3, is to add nanometer iron suspension-s in the aqueous phosphate solution of 10mg/L to concentration, makes that the concentration of nanometer iron is that original ph is respectively 4,6 under the 0.4g/L condition, and 8 o'clock, phosphatic removal effect was as shown in Figure 3.It is thus clear that initial pH is low more, helps PO more
4 3-Removal, when initial pH was 4, the water outlet phosphate concn had all reached below 0.5 mg/L.
Embodiment 6: implementation step is identical with embodiment 3;, initial phosphate concn adds nanometer iron or common iron powder respectively in being the solution of 10mg/L; The concentration of control nanometer iron or common iron powder is 0.4g/L; Contrast adding nanometer iron or common iron powder are to phosphatic removal effect, and the result is that nanometer iron is 78.89% to phosphatic clearance, is higher than common iron powder far away to phosphatic clearance 22.41%.
Claims (3)
1. one kind is utilized adsorption precipitation of nanometer iron and magnetic separation technique to remove phosphatic method in the water, it is characterized in that this method may further comprise the steps:
1) getting absolute ethyl alcohol 100ml in the 500ml there-necked flask, behind the logical argon gas 20min, is the NaBH of 0.4mol/L with 200mL concentration under argon shield
4It is 0.2mol/L FeSO that solution dropwise joins 200ml concentration
4Reaction obtains the nanometer iron suspension-s that concentration is 4.48g/L in the solution;
2) be to add nanometer iron suspension-s in the aqueous phosphate solution of 5 ~ 20mg/L to concentration; The concentration that makes nanometer iron is 0.1 ~ 0.6g/L; Regulate the pH value to 4-8 through dripping hydrochloric acid or sodium hydroxide solution; Under anaerobic in rotating speed is the constant-temperature shaking case of 200 rpm, carry out oscillatory reaction 1-3 h, be statically placed in magnet top 2-3min;
3) solid-liquid separation is taken out supernatant, realizes phosphatic removal in the water body.
2. the method for claim 1 is characterized in that step 2) in, described anaerobic condition is through airtight realization after the argon gas deoxygenation.
3. the method for claim 1 is characterized in that step 2) in, said magnet is diameter 30mm, the disk of thick 10mm, all nanometer iron in the ability absorption reaction.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106111048A (en) * | 2016-07-12 | 2016-11-16 | 成都理工大学 | One is used for removing phosphatic eggshell loaded nano-iron material and preparation method thereof in water |
| CN115925027A (en) * | 2023-03-10 | 2023-04-07 | 湖南国重环境科技有限责任公司 | Pretreatment of water system is failed in antibiotic production of fermentation class |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101182044A (en) * | 2007-11-12 | 2008-05-21 | 浙江大学 | Method for preparing nano ferrite |
| CN101804320A (en) * | 2010-05-04 | 2010-08-18 | 中国科学院生态环境研究中心 | Nano-level iron adsorbent for efficient dephosphorization |
| CN101921016A (en) * | 2010-08-20 | 2010-12-22 | 浙江大学 | Method for removing byproduct bromate of ozone process from water |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101182044A (en) * | 2007-11-12 | 2008-05-21 | 浙江大学 | Method for preparing nano ferrite |
| CN101804320A (en) * | 2010-05-04 | 2010-08-18 | 中国科学院生态环境研究中心 | Nano-level iron adsorbent for efficient dephosphorization |
| CN101921016A (en) * | 2010-08-20 | 2010-12-22 | 浙江大学 | Method for removing byproduct bromate of ozone process from water |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106111048A (en) * | 2016-07-12 | 2016-11-16 | 成都理工大学 | One is used for removing phosphatic eggshell loaded nano-iron material and preparation method thereof in water |
| CN115925027A (en) * | 2023-03-10 | 2023-04-07 | 湖南国重环境科技有限责任公司 | Pretreatment of water system is failed in antibiotic production of fermentation class |
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Application publication date: 20121212 |