CN104307866B - A kind of method that chemical oxidation strengthens chemical leaching restoration of soil polluted by heavy metal - Google Patents
A kind of method that chemical oxidation strengthens chemical leaching restoration of soil polluted by heavy metal Download PDFInfo
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- CN104307866B CN104307866B CN201410276446.7A CN201410276446A CN104307866B CN 104307866 B CN104307866 B CN 104307866B CN 201410276446 A CN201410276446 A CN 201410276446A CN 104307866 B CN104307866 B CN 104307866B
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Abstract
The invention relates to a kind of method that chemical oxidation strengthens chemical leaching restoration of soil polluted by heavy metal, its object is to provide a kind of restorative procedure for strengthening chemical leaching come the chemical oxidation for improving eluent clearance and using for wash-out heavy metal organically combine state, comprise the following steps：Oxidizing agent solution drip washing：Concussion drip washing is carried out using oxidizing agent solution to contaminated soil, leacheate is filtered after centrifugation；Na2EDTA aqueous solution drip washing：Na will be added in the contaminated soil after the oxidizing agent solution drip washing2The EDTA aqueous solution carries out vibration drip washing, and leacheate is filtered after centrifugation.
Description
Technical field
Reparation field is administered the present invention relates to heavy metal pollution of soil, is particularly eluted organic with soil with chemical bond form
The heavy metal of the obligate absorption that matter is combined, the method that the chemical oxidation for being used strengthens chemical leaching.
Background technology
As the event such as " cadmium rice ", " blood lead " takes place frequently, heavy metal pollution of soil harmfulness all the more cause extensively weight
Administer extremely urgent depending on, heavy metal pollution of soil, thus the research on heavy metal soil remediation receives much concern.Wherein, it is biological
The pro-gaze that particularly over-accumulated plant reparation has obtained domestic and international expert with its low cost, environmental protection is repaired, but due to its life
Long period is long, slowly effect, and contaminated concentration, climatic effect be big and super enriching plant species is less, screening process is slow, thus its
Using being extremely restricted；Though the investment of solidification and stabilization technology is smaller, deposited due to that can not separate heavy metal from soil
In potential ecological risk, its application thus be also subject to larger restriction.Elution technique preferably resolves these problems, it
Both can realize that heavy metal was separated from soil, there is instant effect, the advantage of not restricted climatic effect again；The key of elution technique exists
In the selection of eluent, eluent has varied：Inorganic eluent, artificial chelating agent, surfactant, organic acid etc., no
It is very big with eluent difference on effect.Currently, at home and abroad some heavy metal pollution of soil are administered in case and have used elution technique,
But effect on driving birds is not good, in addition to cost, the soil texture, pollution type is limited by, eluent removal efficiency in itself is not high to be also reason
One particularly significant factor；With Na in existing eluent2The chemical leaching effect that EDTA is carried out is most obvious, but by the soil texture and
The influence of pollution type, far can not still be up to state standards value in many actual engineer applieds.
According to the continuous extraction that Tessier is proposed, effect of fertilizer typically can be with occurrence patterns in soil
It is divided into water-soluble state, exchange state, carbonate combine state, Fe-Mn oxide, organically combine state and residual；Europe now uses
The form of heavy metal is divided into 4 kinds i.e. sour solvent, reducible state, oxidable state and residual form by BCR extraction methods, the method.Soil shape
State preservation amount is variant according to soil types (such as soil property, heavy metal species) difference, for most of soil, a huge sum of money
Category residual form proportion is maximum, but because of form stable, be difficult to extract and small to environmental perturbation, the research of this form is less；Remove
Outside residual form, at remaining in several occurrence patterns, with organically combine state (or oxidable state) it is more relative be difficult to be leached agent wash
It is de-.Find that organically combine state (or oxidable state) heavy metal proportion in polluted agricultural land is general in soil through numerous studies
Can 10% or so, when such as Du Xiaolin studies Xiaoqing River, Shandong Province irrigating region Heavy Metal Pattern in Soils, to Cd, Zn, Pb,
Eight kinds of elements such as Cu, Cr are analyzed, and wherein this oxidable state proportion of five kinds of elements is respectively：9.44%,
11.54%, 7.37%, 12.24%, 8.53%；Bend into et al. and to acquire Beijing Chaoyang, Haidian District and Suburb Soil to carrying out
Heavy metal occurrence patterns, wherein between 5.3%-26.8%, Pb is in 0-13.4% for Zn organically combine states proportion
Between；Wang Qifeng shows ten, Guangdong vegetable field soil heavy metal Pb, Cd fractionation results of study, the oxidable state institute of Pb, Cd
It is 10.01%, 7.26% to account for average percent；And in some diggings barren sites, oxidable state proportion can be reached compared with Gao Shui
Flat, Zhu Jiawen has found in western Hunan Huayuan Pb-Zn ore district heavy-metal contaminated soil research bare area：Shared by Pb, Zn, Cd oxidation state
Ratio is up to 43.82%, 22.19%, 32.82% respectively.In a word, this form content is relatively large, and is difficult to elute, thus carries
This occurrence patterns high have particularly significant meaning to drip washing, and the present invention is based on this research for carrying out.
The content of the invention
In soil remediation, chemical oxidizing agent is generally used for organic pollutant degradation；And ground in heavy-metal contaminated soil
In studying carefully, the research for washed off soil heavy metal has no report.The present invention focuses on research eluent and technique, changes medicament kind
Class and consumption, using a kind of oxidating chemicals Fenton reagent solution as Soil leaching agent, auxiliary passes through the high-quality eluent of screening
Na2EDTA (disodium ethylene diamine tetraacetate).The process that the chemical oxidation of heavy metal-polluted soil is extracted is added, soil after drip washing is improved
Heavy metal meltage, to reach the effect of backfill up to standard after drip washing.
This restorative procedure aims to solve the problem that traditional ELUTION METHOD is high to part heavy metal element soil elution rate, after drip washing not
Energy problem up to standard, by eluting the heavy metal of the obligate absorption combined with the soil organism with chemical bond form, and and drip washing
The method that agent is combined.
To reach above repairing effect, the present invention strengthens chemical leaching restoration of soil polluted by heavy metal for a kind of chemical oxidation
Method, comprise the following steps：
Aqueous oxidizing agent solution drip washing：Concussion drip washing is carried out using aqueous oxidizing agent solution to contaminated soil, pouring is filtered after centrifugation
Washing lotion；
Na2EDTA aqueous solution drip washing：Na will be added in the contaminated soil after the aqueous oxidizing agent solution drip washing2EDTA
The aqueous solution carries out vibration drip washing, and leacheate is filtered after centrifugation.
Wherein described Na2Also include the step of addition clear water carries out vibration drip washing after EDTA aqueous solution drip washing, after centrifugation
Filter leacheate.
The compound concentration of wherein described Fenton reagent aqueous solution is, FeSO4·7H2O dosages are 24g/L, H2O2(30%)
Dosage is 200ml/L, and pH regulations are arrived into 3-4.
Wherein described aqueous oxidizing agent solution is with the contaminated soil liquid-solid ratio scope 5：1 to 15:Between 1, preferably 10:1；
The Na2The EDTA aqueous solution is with the contaminated soil liquid-solid ratio scope 5：1 to 15:Between 1, preferably 10:1.
Solution 0.1mol/L C in wherein described aqueous oxidizing agent solution rinsing step6H8O7Tune pH is 3-4, preferably 3.
Wherein described Na2Solution is adjusted with 0.1mol/L HCl or 0.1mol/LNaOH solution in EDTA aqueous solution rinsing steps
PH be 3.9-8 between, preferably 4.5.
The wherein described aqueous oxidizing agent solution drip washing time is 0.5-2 hours, preferably 1 hour；The Na2The EDTA aqueous solution drenches
The time is washed for 0.5-2 hours, preferably 1 hour.
By above-mentioned technical proposal, the present invention at least has following technique effect：
1st, the heavy metal Main Morphology of existing eluent removal concentrates on easy solvent and exchange state, to being difficult to what is be eluted
Eluted combination state removal effect is poor, often leads to clearance not high；With oxidant and eluent substep drip washing, further carry
Heavy metal-polluted soil elution efficiency high, reduces ecological risk.
2nd, Iron in Soil oxide greatly reduces the activity of residual heavy metal in soil after drip washing, forces heavy metal in soil
Further stablize in earth.This can cause new unformed or microstructure mainly due in lessivation during new oxide generation
Generation, a large amount of adsorbing metal ions or ion cluster；Ferriferous oxide occur Forms Transformation, heavy metal with its may occur precipitation and
Co-precipitation, ultimately results in and does not elute heavy metal activity in soil and substantially reduce.
Specific embodiment
With reference to embodiments, drip washing is carried out by three kinds of different heavy metal concentration Polluted Soils, it is above-mentioned to the present invention
It is described in more detail with other technical characteristic and advantage.
Embodiment 1
The collection Soil Surrounding of somewhere mining area 1, surveys its basic physical and chemical：Cadmium：1.34mg/kg, lead：383mg/kg, zinc：
313mg/kg, pH=6.1, adopted soil is air-dried at room temperature, and sieves particle diameter soil between 60 mesh -200 mesh, is filled
Divide and stir；
(1) weigh 10g soil to be put into 250ml triangular flasks, add 50ml0.5mol/L Na2The EDTA aqueous solution, uses
0.1mol/L HCl adjust pH to 4, horizontal hunting speed of room temperature be 200rpm under vibrate 50min, be centrifuged, isolate soil and
Leacheate；
(2) the 0.5mol/L Na of 50ml are added2The EDTA aqueous solution, adjusts pH to 4, in room temperature with 0.1mol/L HCl
Horizontal oscillations speed is centrifuged to vibrate 50min under 200rpm, isolates soil and leacheate；
(3) soil after being centrifuged again, adds the deionized water of 50ml, in the case where horizontal hunting speed of room temperature is 200rpm
Soil and leacheate are isolated in vibration 1h, centrifugation.
Embodiment 2
The collection Soil Surrounding of somewhere mining area 1, surveys its basic physical and chemical：Cadmium：1.34mg/kg, lead：383mg/kg, zinc：
313mg/kg, pH=6.1, adopted soil is air-dried at room temperature, and sieves particle diameter soil between 60 mesh -200 mesh, is filled
Divide and stir；
(1) weigh 10g soil to be put into 250ml triangular flasks, (compound concentration is 24g/ to add 50ml Fenton reagent aqueous solutions
L FeSO4·7H2O, 200ml/L H2O2, use 0.1mol/L C6H8O7PH is to 3) for regulation, is in horizontal hunting speed of room temperature
50min is vibrated under 200rpm, is centrifuged, isolate soil and leacheate；
(2) soil after being centrifuged, adds 50ml0.5mol/L Na2The EDTA aqueous solution, with 0.1mol/L HCl adjust pH to
4,50min is vibrated in the case where horizontal hunting speed of room temperature is 200rpm, it is centrifuged, isolate soil and leacheate；
(3) soil after being centrifuged again, adds the deionized water of 50ml, in the case where horizontal hunting speed of room temperature is 200rpm
Soil and leacheate are isolated in vibration 1h, centrifugation.
After the Step gragient elution of embodiment 1 and 2 two groups of samples more than, after oxidation drip washing is increased after measured, in embodiment 2
Cd, Pb, Zn in soil content be respectively 0.45mg/kg, 217mg/kg, 178mg/kg.Only used relative in example 1
Na2Heavy metal content in soil value 0.61mg/kg, 266mg/kg, 210mg/kg after EDTA aqueous solution drip washing, are respectively increased
12.1%th, 22.8% and 10.2%, clearance has reached 66.4%, 53.5% and 32.9%.Heavy metal-polluted soil Pb, Zn after drip washing
Content reaches soil environment quality value secondary standard, and Cd reaches standard of soil environment quality value grade III Standard.
Embodiment 3
The collection Soil Surrounding of somewhere mining area 1, surveys its basic physical and chemical：Cadmium：1.34mg/kg, lead：383mg/kg, zinc：
313mg/kg, pH=6.1, adopted soil is air-dried at room temperature, and sieves particle diameter soil between 60 mesh -200 mesh, is filled
Divide and stir；
(1) weigh 10g soil to be put into 250ml triangular flasks, add 100ml0.5mol/L Na2The EDTA aqueous solution, uses
0.1mol/L HCl adjust pH to 5, and 1h is vibrated in the case where horizontal hunting speed of room temperature is 200rpm, are centrifuged, and isolate soil and pouring
Washing lotion；
(2) the 0.5mol/L Na of 100ml are added2The EDTA aqueous solution, adjusts pH to 5, in room temperature with 0.1mol/L HCl
Horizontal oscillations speed is centrifuged to vibrate 1h under 200rpm, isolates soil and leacheate；
(3) soil after being centrifuged again, adds the deionized water of 100ml, is 200rpm in horizontal hunting speed of room temperature
Lower vibration 1h, centrifugation, isolates soil and leacheate.
Embodiment 4
The collection Soil Surrounding of somewhere mining area 1, surveys its basic physical and chemical：Cadmium：1.34mg/kg, lead：383mg/kg, zinc：
313mg/kg, pH=6.1, adopted soil is air-dried at room temperature, and sieves particle diameter soil between 60 mesh -200 mesh, is filled
Divide and stir；
(1) weigh 10g soil to be put into 250ml triangular flasks, (compound concentration is to add 100ml Fenton reagent aqueous solutions
24g/L FeSO4·7H2O, 200ml/L H2O2, use 0.1mol/L C6H8O7PH is to 3.5) for regulation, in horizontal hunting speed of room temperature
To vibrate 1h under 200rpm, soil and leacheate are isolated in centrifugation；
(2) soil after being centrifuged, adds 100ml0.5mol/L Na2The EDTA aqueous solution, with 0.1mol/LHCl adjust pH to
5,1h is vibrated in the case where horizontal hunting speed of room temperature is 200rpm, it is centrifuged, isolate soil and leacheate；
(3) soil after being centrifuged again, adds the deionized water of 100ml, is 200rpm in horizontal hunting speed of room temperature
Lower vibration 1h, centrifugation, isolates soil and leacheate.
After the Step gragient elution of embodiment 3 and 4 two groups of samples more than, after oxidation drip washing is increased after measured, in embodiment 4
Cd, Pb, Zn in soil content be respectively 0.37mg/kg, 181mg/kg, 166mg/kg.Only used relative in example 3
Na2Heavy metal content in soil value 0.54mg/kg, 250mg/kg, 201mg/kg after EDTA aqueous solution drip washing, are respectively increased
12.7%th, 18.0% and 11.2%, clearance has reached 72.4%, 52.7% and 47.0%.Heavy metal-polluted soil Pb, Zn after drip washing
Content reaches soil environment quality value secondary standard, and Cd reaches standard of soil environment quality value grade III Standard.
Embodiment 5
Certain contaminated soil of severe mining area 2 is gathered, its basic physical and chemical is surveyed：Cadmium：4.19mg/kg, lead：761mg/kg, zinc：
493mg/kg, pH=7.06, adopted soil is air-dried at room temperature, and sieves particle diameter soil between 60 mesh -200 mesh, is filled
Divide and stir；
(1) weigh 10g soil to be put into 250ml triangular flasks, add the 0.5mol/L Na of 150ml2The EDTA aqueous solution, uses
0.1mol/L HCl adjust pH to 6.5, horizontal hunting speed of room temperature be 200rpm under vibrate 2h, be centrifuged, isolate soil and
Leacheate；
(2) the 0.5mol/L Na of 150ml are added2The EDTA aqueous solution, adjusts pH to 6.5, in room with 0.1mol/L HCl
The flat hunting speed of warm water is centrifuged to vibrate 2h under 200rpm, isolates soil and leacheate；
(3) soil after being centrifuged again, adds the deionized water of 150ml, is 200rpm in horizontal hunting speed of room temperature
Lower vibration 1h, centrifugation, isolates soil and leacheate.
Embodiment 6
Certain contaminated soil of severe mining area 2 is gathered, its basic physical and chemical is surveyed：Cadmium：4.19mg/kg, lead：761mg/kg, zinc：
493mg/kg, pH=7.06, adopted soil is air-dried at room temperature, and sieves particle diameter soil between 60 mesh -200 mesh, is filled
Divide and stir；
(1) weigh 10g soil to be put into 250ml triangular flasks, add 150ml certain concentrations Fenton reagent aqueous solution (to prepare
Concentration is 24g/L FeSO4·7H2O, 200ml/L H2O2, use 0.1mol/L C6H8O7Solution adjusts pH to 4), in room temperature level
Hunting speed is centrifuged to vibrate 2h under 200rpm, isolates soil and leacheate；
(2) soil after being centrifuged, adds 150ml0.5mol/L Na2The EDTA aqueous solution, pH is adjusted with 0.1mol/L HCl
To 6.5,2h is vibrated in the case where horizontal hunting speed of room temperature is 200rpm, be centrifuged, isolate soil and leacheate；
(3) soil after being centrifuged again, adds the deionized water of 150ml, is 200rpm in horizontal hunting speed of room temperature
Lower vibration 1h, centrifugation, isolates soil and leacheate.
After Step gragient elution of the 6 two groups of samples of embodiment 5 and embodiment more than, after measured, embodiment 5 increases oxidation and drenches
Cd, Pb, Zn clearance after washing only uses Na with respect to embodiment 62EDTA aqueous solution drip washing clearances increased 4.93%,
9.05%th, 12.5%, the clearance of Cd, Pb, Zn concentration has respectively reached 76.6%, 89.4%, 80.2% after drip washing oxidation.Through
After drip washing, Pb, Zn are up to state standards soil environment quality value secondary standard, and Cd reaches grade III Standard.Embodiment 1-
2nd, in 3-4 and 5-6, under the conditions of the eluent is using different pH, duration of oscillation, solid-to-liquid ratio within right etc.
Achieve preferable drip washing effect.
According to soil is how many, type and drip washing quality requirement can suitably adjust aqueous oxidizing agent solution in contaminated soil lessivation
Liquor concentration, Na2PH value of solution in EDTA concentration of aqueous solution, leacheate and contaminated soil liquid-solid ratio, each rinsing step, during drip washing
Between etc., to realize optimal repairing effect.
Embodiment described above is only that the preferred embodiment of the present invention is described, not to model of the invention
Enclose and be defined, on the premise of design spirit of the present invention is not departed from, those of ordinary skill in the art are to technical side of the invention
Various modifications and improvement that case is made, all should fall into the protection domain of claims of the present invention determination.
Claims (7)
1. a kind of method that chemical oxidation strengthens chemical leaching restoration of soil polluted by heavy metal, it is characterised in that comprising following step
Suddenly：
Aqueous oxidizing agent solution drip washing：Concussion drip washing is carried out using aqueous oxidizing agent solution to contaminated soil, leacheate is filtered after centrifugation；
Wherein described aqueous oxidizing agent solution is Fenton reagent solution；
The Fenton reagent solution compound concentration is FeSO4·7H2O dosages are 24g/L, 30% H2O2Dosage is 200ml/
L, and 3-4 is arrived into pH regulations；
The aqueous oxidizing agent solution is with the contaminated soil liquid-solid ratio scope 5：1 to 15:Between 1；
The aqueous oxidizing agent solution pH 0.1mol/L C6H8O7Adjust to 3-4；
Na2EDTA aqueous solution drip washing：Na will be added in the contaminated soil after the aqueous oxidizing agent solution drip washing2EDTA is water-soluble
Liquid carries out vibration drip washing, and leacheate is filtered after centrifugation；
The Na2EDTA concentration of aqueous solution is 0.1-1mol/L；
The Na2The EDTA aqueous solution is with the contaminated soil liquid-solid ratio scope 5：1 to 15:Between 1；
The Na2PH value of solution is adjusted to 3.9- with the NaOH of 0.1mol/L HCl or 0.1mol/L in EDTA aqueous solution rinsing steps
8；
The aqueous oxidizing agent solution drip washing time is 0.5-2 hours；The Na2The EDTA aqueous solution drip washing times are 0.5-2 hours.
2. the method that chemical oxidation as claimed in claim 1 strengthens chemical leaching restoration of soil polluted by heavy metal, its feature exists
In：The Na2Also include the step of addition clear water carries out vibration drip washing after EDTA aqueous solution drip washing, drip washing is filtered after centrifugation
Liquid.
3. the method that chemical oxidation as claimed in claim 1 strengthens chemical leaching restoration of soil polluted by heavy metal, its feature exists
In：The Na2EDTA concentration of aqueous solution is 0.5mol/L.
4. the method that chemical oxidation as claimed in claim 1 strengthens chemical leaching restoration of soil polluted by heavy metal, its feature exists
In：The aqueous oxidizing agent solution is 10 with the contaminated soil liquid-solid ratio:1；The Na2The EDTA aqueous solution and the contaminated soil
Liquid-solid ratio is 10:1.
5. the method that chemical oxidation as claimed in claim 1 strengthens chemical leaching restoration of soil polluted by heavy metal, its feature exists
In：The aqueous oxidizing agent solution pH 0.1mol/L C6H8O7Adjust to 3.
6. the method that chemical oxidation as claimed in claim 1 strengthens chemical leaching restoration of soil polluted by heavy metal, its feature exists
In：The Na2PH value of solution is adjusted to 4.5 with 0.1mol/L HCl in EDTA aqueous solution rinsing steps.
7. the method that chemical oxidation as claimed in claim 1 strengthens chemical leaching restoration of soil polluted by heavy metal, its feature exists
In：The aqueous oxidizing agent solution drip washing time is 1 hour；The Na2The EDTA aqueous solution drip washing times are 1 hour.
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| CN105855286A (en) * | 2016-04-05 | 2016-08-17 | 南京农业大学 | Oxidation removing method for polycyclic aromatic hydrocarbon in soil through Fenton reagent bag |
| CN106623405A (en) * | 2016-12-22 | 2017-05-10 | 常州大学 | Method for remediation of benzene hexachloride contaminated soil by Fe (II) / CaO2 |
| CN107008747A (en) * | 2017-05-27 | 2017-08-04 | 山东师范大学 | A kind of microwave reinforced oxidation elution combined remediation method in pollution of chromium place |
| CN109351768A (en) * | 2018-11-14 | 2019-02-19 | 中国石油大学(华东) | A kind of method of chemical oxidation and chemical leaching renovation of heavy metal polluted soil with combined |
| CN111672898B (en) * | 2020-06-30 | 2022-04-01 | 南京浦世环境科技发展有限公司 | Chemical leaching method for heavy metal contaminated soil |
| CN112453041A (en) * | 2020-11-03 | 2021-03-09 | 武汉科技大学 | Soil heavy metal eluting agent, eluting method of heavy metal contaminated soil and application |
| CN112718840A (en) * | 2021-01-19 | 2021-04-30 | 湖南平安环保股份有限公司 | Treatment method of heavy metal-organic matter composite contaminated soil |
| CN114275984B (en) * | 2021-12-22 | 2023-03-21 | 华中科技大学 | Electrochemical leaching lead recovery method for lead-containing sludge |
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| US5286141A (en) * | 1993-02-12 | 1994-02-15 | Vigneri Ronald J | Method and system for remediation of groundwater contamination |
| US6623211B2 (en) * | 2000-05-24 | 2003-09-23 | Rutgers University | Remediation of contaminates including low bioavailability hydrocarbons |
| JP2012239952A (en) * | 2011-05-17 | 2012-12-10 | National Agriculture & Food Research Organization | Fenton reaction catalyst produced by using reducing organic substance as raw material |
| CN102950149A (en) * | 2012-05-15 | 2013-03-06 | 武汉市华鑫源环境科技有限公司 | Restoration method for organic contaminated soil |
| CN102784452B (en) * | 2012-07-18 | 2015-11-04 | 广西大学 | A kind of heavy metal stabilizer for removal heavy metal pollution and using method thereof |
| CN103008338A (en) * | 2012-11-26 | 2013-04-03 | 苏州科技学院 | Repair method of dipterex pesticide contaminated soil |
| CN103611725B (en) * | 2013-11-20 | 2016-04-06 | 北京鼎实环境工程有限公司 | A kind of electronation combines with chemical leaching the method for restoration of soil polluted by heavy metal |
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