CN108529799A - The method that photodissociation network strengthens heavy metal complexing waste water reclaiming - Google Patents
The method that photodissociation network strengthens heavy metal complexing waste water reclaiming Download PDFInfo
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- CN108529799A CN108529799A CN201810369780.5A CN201810369780A CN108529799A CN 108529799 A CN108529799 A CN 108529799A CN 201810369780 A CN201810369780 A CN 201810369780A CN 108529799 A CN108529799 A CN 108529799A
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- heavy metal
- waste water
- photodissociation
- metal complexing
- ion
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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
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
-
- 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
- C02F2101/20—Heavy metals or heavy metal compounds
-
- 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
Abstract
The invention discloses a kind of photodissociation networks to strengthen the method that waste water reclaiming is complexed in heavy metal, is as follows：After complexing waste water containing target heavy metal is filtered processing, ferron is added and carries out Air Exposure；The water outlet of step (1) is pumped into progress photocatalysis decomplexing in Photoreactor；The water outlet of step (2) is pumped into the I grade adsorption columns of filling A class adsorbents, recycles target heavy metal ion；The water outlet of step (3) is pumped into the II grade adsorption columns of loaded resin B class adsorbents, extracts ferric ion；After the adsorption column in step (4) penetrates, into II grades of adsorption columns being pumped into regenerative agent is regenerated, and recycles desorption liquid containing ferric ion；The present invention is strengthened by the integration of photocatalysis decomplexing and the integrated control of selective absorption technique, realize the Selective Separation of heavy metal ion and additional Fe (III) ion, the recycling of heavy metal and recycling for iron are realized, medicine consumption and energy consumption are significantly reduced.
Description
Technical field
The present invention relates to a kind of photodissociation networks to strengthen the method that waste water reclaiming is complexed in heavy metal, belongs to field of waste water treatment.
Background technology
Complex state heavy metal has extensive presence in natural water body and industrial water body.NOM and DOM are more in natural water body
Contain the ligand functional groups such as hydroxyl, amino and carboxyl, it is easy to form soluble heavy metal chelate with heavy metal, prevent
Deposition of the heavy metal ion in natural water body.In order to ensure quality of coating in electroplating process, need to add into plating solution big
Complexing agent is measured, heavy metal out of electroplating wastewater is caused mostly to exist with complex state.In the presence of inorganic or organic ligand, heavy metal moves
Shifting ability is enhanced, and can be promoted bio-absorbable and be increased the enrichment degree of heavy metal.Therefore, compared to an ionic state huge sum of money
Belong to, the influence bigger that the heavy metal of complex state can bring aquatile.Therefore, a complex state huge sum of money how is simply and effectively removed
Category has become heavy metal containing wastewater treatment field strategic point problem to be solved.
Compared to ionic state heavy metal, complex state heavy metal has because it is complexed to surround to be formed by coordination atoms such as multiple N or O
The very multiple tooth chelate of the single or multiple core of high stability coefficient, make its be difficult to by traditional coagulating sedimentation, chemical precipitation and
The methods of ion exchange removes.Chelating absorption method has preferable Selective Separation effect to free heavy metal ion, but right
The Selective Separation effect of the heavy metal of complex state is poor, this is because complexing agent wraps up heavy metal ion wherein, fully takes up
Its coordination site so that can not effective as selective position adsorbing separation.The Selective Separation for realizing heavy metal, this requires
It needs to carry out decomplexing to complex state heavy metal.At present decomplexing technology according to decomplexing principle can be divided into ligand displacement decomplexing technology,
Ligand aoxidizes decomplexing technology and metal ion restores decomplexing technology.
Ligand displacement decomplexing technology is to displace a target huge sum of money by addition and the stronger metal ion of ligand complex ability
Belong to ion, to realize heavy metal decomplexing.Ligand oxidation decomplexing technology is by non-oxidizing ligand compound, and it is funeral to make ligand transformations
The product of complexing power or the mode of permineralization ligand compound are lost, abolishing complexing makes heavy metal ion separate out.And it is golden
Belong to ion reduction decomplexing technology be by reproducibility reagent by the heavy metal ion of complexing be reduced to lower valency metal ion or
Person's metal simple-substance reduces the stability of its complex compound, to realize that complex state heavy metal takes off steady decomplexing.These methods are in processing network
Closing on state heavy metal has more significant effect.But no matter ligand displacement decomplexing or ligand aoxidize decomplexing and all there is medicament and disappear
Consumption is big, and waste production is big, the extensive feature of technology；And metal ion reduction decomplexing technology still remain recycling metal purity it is low
Problem.
Therefore, seek a kind of decomplexing coupling heavy metal selective recovery technology of intensive style, it has also become contemporary society develops
Demand.Based on this thinking, it is proposed that a kind of next Fe (III) ions and O2Promote light-catalysed intensive decomplexing technology altogether,
Realize recycling and target heavy metal selective recovery for Fe (III) ion.
Invention content
The present invention is directed to the deficiencies in the prior art, provides photodissociation network and strengthens heavy metal complexing waste water reclaiming
Method, to solve problems of the prior art.
The present invention relates to photodissociation networks to strengthen the method that waste water reclaiming is complexed in heavy metal, is specifically namely based on Fe
(III) ion and O2Promote photocatalysis decomplexing altogether and abolish interference of the organic acid complexing agent to heavy metal adsorption, is inhaled to strengthen chelating
The attached dose of selective absorption to target heavy metal ion realizes that lower heavy metal low cost recycling coexists in organic acid.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of method that photodissociation network strengthens heavy metal complexing waste water reclaiming, is as follows：
(1) it pre-processes：After complexing waste water containing target heavy metal is filtered processing, ferron is added and is exposed
Gas disposal；Fe (III) ion of addition play ligand displacement decomplexing and photocatalysis decarboxylation dual function, expose into oxygen play
Enhance the effect of photochemistry decarboxylation；
(2) photocatalysis decomplexing：The water outlet of step (1) is pumped into progress photocatalysis decomplexing in Photoreactor；
The technical principle of the above process is shown below：
Cu(II)-EDTA+Fe(III)-→Fe(III)-EDTA+Cu(II) (1-1)
4Fe(II)+4H++O2→4Fe(III)+2H2O (1-4)
(3) heavy metal recovery：The water outlet of step (2) is pumped into the I grade adsorption columns of filling A class adsorbents, recycles target weight
Metal ion；The adsorbent that there is highly selective separation to target heavy metal ion has wherein been loaded, selective suction is passed through
Attached recycling target heavy metal ion；
(4) iron recycles：The water outlet of step (3) is pumped into the II grade adsorption columns of filling B class adsorbents, wherein having loaded to Fe
(III) ion has the adsorbent of efficient selective separation, extracts ferric ion；
(5) ferrikinetics utilizes：After the adsorption column in step (4) penetrates, regenerative agent progress is pumped into II grades of adsorption columns
Desorption liquid containing ferric ion is recycled in regeneration.
As an improvement of the present invention, the heavy metal complexing waste water described in the step (1) refers to containing organic acid
The heavy metal wastewater thereby of complexing agent, wherein organic acid complexing agent refer to the organic acid containing carboxyl, preferably ammonia in its molecular structure
The EDTA of yl carboxylic acid class, the citric acid of hydroxycarboxylic acid.
As an improvement of the present invention, the ferron in the step (1) is ferric salt solution, the trivalent iron salt
Solution is ferric chloride solution, ferrum sulfuricum oxydatum solutum or iron nitrate solution, and iron concentration is 0.1-1.0mol/L in the ferron.
As an improvement of the present invention, the molar concentration of ferron is attached most importance in metal complex waste water in the step (1)
0.1-1.0 times of complexing agent molar concentration.
As an improvement of the present invention, aeration mode is air aeration in the step (1)；It is exposed in the step (1)
Dissolved oxygen concentration after gas in heavy metal complexing waste water is 8.0mg/L or more at normal temperatures.
As an improvement of the present invention, waterpower of the heavy metal complexing waste water in Photoreactor is stopped in the step (2)
It is 10-60min to stay the time.
As an improvement of the present invention, in the step (2), the light source effective wavelength of Photoreactor is 200-420nm,
The light source of the Photoreactor is mercury lamp.
As an improvement of the present invention, the A class adsorbents in the step (3) are chelate sorbent, and the chelating is inhaled
Attached dose is amino carboxylic acid resinoid D463, pyridine resinoid TP22, pyridines resin M 4195, phosphoramidic-resin Purolite
Any one in S950 or amidoxim resin Purolite S910.
As an improvement of the present invention, target heavy metal ion is in cobalt, copper, zinc, cadmium and lead in the step (1)
It is one or more.
As an improvement of the present invention, the B class adsorbents in the step (4) are phosphono and sulfonic resinoid Purolite
S957。
As an improvement of the present invention, the regenerative agent in the step (5) refer to 2%-20%wt dilute sulfuric acid or
The dust technology of 5%-20%wt dilute hydrochloric acid or 5%-20%wt.
As a result of the above technology, the present invention compared with the prior art, has the advantage that as follows：
(1) pass through Fe (III) ions and O2Promote photocatalysis decomplexing altogether, substantially reduce the water conservancy residence time of photodissociation network,
Effectively save the energy；
(2) it uses high-selectivity adsorption agent to recycle Fe (III) ion, then is used as by reground resin desorption liquid and adds iron examination
Agent realizes the recycling of photocatalysis medicament, reduces dependence of the decomplexing technology to reagent consumption amount significantly；
(3) recycling of the high-selectivity adsorption agent to target heavy metal ion is enhanced by photocatalysis decomplexing, improved back
The purity for receiving metal, realizes effective recycling of resource, increases the economic value of technology.
Description of the drawings
Fig. 1 is the comparison diagram of chelating absorption resin performance before and after decomplexing；
Specific implementation mode
With reference to embodiment, the present invention is furture elucidated.
Embodiment：Waste water is complexed in Cu-EDTA heavy metals
The first step, pretreatment, photocatalysis decomplexing：To the Cu-EDTA heavy metals of 1.0L complexing waste water, (wherein, Cu (II) is dense
Degree is 1.0mmol/L, typical a concentration of 2.0mmol/L of complexing agent EDTA) in add ferron, and maintain Cu-EDTA complexings useless
The pH of water is between 2.0-4.0, then is complexed in waste water and is exposed into air to Cu-EDTA heavy metals so that molten in the waste water after aeration
Solution oxygen concentration reaches 8.0mg/L or more at normal temperatures.The waste water after aeration is pumped into using 300W mercury lamps as light source again, light source is effective
Photocatalysis decomplexing is carried out in the Photoreactor that wavelength is 200-420nm.EDTA resolution ratios under several groups of decomplexing parameters in contrast table 1,
It can be found that Fe (III) ions and O2The decomposition to EDTA can preferably be realized by promoting photodissociation network technology altogether.
1 decomplexing process control parameters of table and its decomplexing effect
Second step, heavy metal recovery：Waste water is complexed (according to the decomplexing item of serial number 5 in Cu-EDTA heavy metals after photodissociation network
Waste water is complexed in part, the Cu-EDTA heavy metals that EDTA resolution ratios are 98.7%), it is that 1.0g/L is added separately to fill according to solid-to-liquid ratio
There are amino carboxylic acid resinoid D463, phosphoramidic-resin PuroliteS950, pyridine resinoid TP220, pyridines resin M 4195
Or in the I grade adsorption columns of amidoxim resin PuroliteS910, and maintain the pH of Cu-EDTA heavy metals complexing waste water after photodissociation network
It between 5.0-7.0, is placed in the constant temperature oscillator under 298K, controls rotating speed 160rpm, fully oscillation absorption for 24 hours, is inhaled
Waste water is complexed in Cu-EDTA heavy metals after attached Cu (II).From fig. 1, it can be seen that under the same terms before and after decomplexing chelating resin to Cu
(II) absorption property is it can be found that several chelating resins have significant increase to the absorption property of Cu (II) after decomplexing.
Iron recycles：Waste water is complexed in Cu-EDTA heavy metals after Adsorption of Cu (II), is that 1.0g/L adds respectively according to solid-to-liquid ratio
Enter to the II grade adsorption columns equipped with phosphono and sulfonic base resin Purolite S957, and maintain the pH of the waste water between 5.0-7.0,
It is placed in the constant temperature oscillator under 298K, controls rotating speed 160rpm, fully oscillation is adsorbed for 24 hours, and is carried out to Fe (III) rate of recovery
Detection.Compare the following table 2 in Fe (III) ion the rate of recovery it is found that Purolite S957 to Fe (III) ion have it is beneficial
Recovering effect.
2 iron recovering effect of table
Third walks, and ferrikinetics utilizes：To adsorb the S957 resins after Fe (III) ion (according to the decomplexing condition of serial number 14,
Fe (III) rate of recovery is the B classes adsorbent after 98.0% absorption), it is regenerated using different regenerative agents.Compare following table
Fe (III) ion desorption rates in 3 are it can be found that the Fe (III) of S957 resin adsorptions has preferable desorption rate.
Regeneration effect of the different regenerative agents of table 3 to S957
To serial number 19, the desorption liquid that Fe (III) desorption rate is 90.8% is detected, it is known that the composition of desorption liquid：0.1-
Fe (III) ion of 0.25mol/L, the hydrogen ion of 0.5-1.0mol/L and a small amount of EDTA decomposition products, 300-1000mg
(TOC)/L.Add Cu-EDTA heavy metals as ferron and waste water be complexed, and maintain the pH of the waste water 1.5-3.5 it
Between, the resolution ratio of EDTA in contrast table 4, it can be found that desorption liquid can also realize the decomposition to EDTA as ferron.
Decomplexing effect of 4 desorption liquid of table as ferron
Above-described embodiment is only the preferred technical solution of the present invention, and is not construed as the limitation for the present invention, the present invention
Protection domain should with claim record technical solution, including claim record technical solution in technical characteristic etc.
It is protection domain with alternative, i.e., equivalent replacement within this range is improved, also within protection scope of the present invention.
Claims (10)
1. a kind of method that photodissociation network strengthens heavy metal complexing waste water reclaiming, which is characterized in that be as follows：
(1) it pre-processes：After complexing waste water containing target heavy metal is filtered processing, ferron is added and carries out at aeration
Reason；
(2) photocatalysis decomplexing：The water outlet of step (1) is pumped into progress photocatalysis decomplexing in Photoreactor；
(3) heavy metal recovery：The water outlet of step (2) is pumped into the I grade adsorption columns of filling A class adsorbents, recycles target heavy metal
Ion；
(4) iron recycles：The water outlet of step (3) is pumped into the II grade adsorption columns of filling B class adsorbents, extracts ferric ion；
(5) ferrikinetics utilizes：After the adsorption column in step (4) penetrates, into II grades of adsorption columns being pumped into regenerative agent is regenerated,
Recycle desorption liquid containing ferric ion.
2. the method that a kind of photodissociation network according to claim 1 strengthens heavy metal complexing waste water reclaiming, it is characterised in that：
Ferron in the step (1) is ferric salt solution, the ferric salt solution be ferric chloride solution, ferrum sulfuricum oxydatum solutum or
Iron nitrate solution, iron concentration is 0.1-1.0mol/L in the ferron.
3. the method that a kind of photodissociation network according to claim 1 strengthens heavy metal complexing waste water reclaiming, it is characterised in that：
The molar concentration of ferron is attached most importance to 0.1-1.0 times of metal complex waste water complexing agent molar concentration in the step (1).
4. the method that a kind of photodissociation network according to claim 1 strengthens heavy metal complexing waste water reclaiming, it is characterised in that：
Aeration mode is air aeration in the step (1)；Dissolved oxygen in the step (1) after aeration in heavy metal complexing waste water is dense
Degree is 8.0mg/L or more at normal temperatures.
5. the method that a kind of photodissociation network according to claim 1 strengthens heavy metal complexing waste water reclaiming, it is characterised in that：
Hydraulic detention time of the heavy metal complexing waste water in Photoreactor is 10-60min in the step (2).
6. the method that a kind of photodissociation network according to claim 1 strengthens heavy metal complexing waste water reclaiming, it is characterised in that：
In the step (2), the light source effective wavelength of Photoreactor is 200-420nm.
7. the method that a kind of photodissociation network according to claim 1 strengthens heavy metal complexing waste water reclaiming, it is characterised in that：
A class adsorbents in the step (3) are chelate sorbent, and the chelate sorbent is amino carboxylic acid resinoid D463, pyridine
Resinoid TP22, pyridines resin M 4195, phosphoramidic-resin Purolite S950 or amidoxim resin Purolite S910
In any one.
8. the method that a kind of photodissociation network according to claim 1 strengthens heavy metal complexing waste water reclaiming, it is characterised in that：
Target heavy metal ion is one or more in cobalt, copper, zinc, cadmium and lead in the step (1).
9. the method that a kind of photodissociation network according to claim 1 strengthens heavy metal complexing waste water reclaiming, it is characterised in that：
B class adsorbents in the step (4) are phosphono and sulfonic resinoid Purolite S957.
10. the method that a kind of photodissociation network according to claim 1 strengthens heavy metal complexing waste water reclaiming, feature exist
In：Regenerative agent in the step (5) refers to the dilute sulfuric acid or 5%-20%wt dilute hydrochloric acid or 5%-20%wt of 2%-20%wt
Dust technology.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810369780.5A CN108529799A (en) | 2018-04-21 | 2018-04-21 | The method that photodissociation network strengthens heavy metal complexing waste water reclaiming |
| PCT/CN2018/103158 WO2019200811A1 (en) | 2018-04-21 | 2018-08-30 | Method for enhancing recycling of heavy metal complex wastewater by means of photo-decomplexing |
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| CN201810369780.5A CN108529799A (en) | 2018-04-21 | 2018-04-21 | The method that photodissociation network strengthens heavy metal complexing waste water reclaiming |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104108819A (en) * | 2014-06-13 | 2014-10-22 | 南京大学 | A combined process for treating heavy metal complexing waste water |
| CN104129831A (en) * | 2014-07-29 | 2014-11-05 | 南京大学 | Method for simultaneous removal and recovery of heavy metal ions and organic acid by using chelating resin |
| CN105692768A (en) * | 2016-03-31 | 2016-06-22 | 南京大学 | Method for selectively extracting heavy metals in heavy metal-ammonia complexing wastewater by virtue of chelate resin |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013040389A1 (en) * | 2011-09-14 | 2013-03-21 | University Of South Florida | Cactus mucilage and ferric ions for the removal of arsenate (as(v)) from water |
| CN103241803A (en) * | 2013-05-14 | 2013-08-14 | 广东新大禹环境工程有限公司 | Electroplating wastewater separating process |
| US9193608B2 (en) * | 2013-07-15 | 2015-11-24 | King Fahd University Of Petroleum And Minerals | Removal of heavy metals from aqueous solutions using vanadium-doped titanium dioxide nanoparticles |
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- 2018-04-21 CN CN201810369780.5A patent/CN108529799A/en active Pending
- 2018-08-30 WO PCT/CN2018/103158 patent/WO2019200811A1/en active Application Filing
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104108819A (en) * | 2014-06-13 | 2014-10-22 | 南京大学 | A combined process for treating heavy metal complexing waste water |
| CN104129831A (en) * | 2014-07-29 | 2014-11-05 | 南京大学 | Method for simultaneous removal and recovery of heavy metal ions and organic acid by using chelating resin |
| CN105692768A (en) * | 2016-03-31 | 2016-06-22 | 南京大学 | Method for selectively extracting heavy metals in heavy metal-ammonia complexing wastewater by virtue of chelate resin |
Non-Patent Citations (1)
| Title |
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| ZHE XU ETC.: "A new combined process for efficient removal of Cu(II) organic complexes from wastewater: Fe(III) displacement/UV degradation/alkaline precipitation", 《WATER RESEARCH》 * |
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