CN104307866A - Method for repairing soil polluted by heavy metals by using chemical oxidation enhanced chemical leaching - Google Patents
Method for repairing soil polluted by heavy metals by using chemical oxidation enhanced chemical leaching Download PDFInfo
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Abstract
The invention relates to a method for repairing soil polluted by heavy metals by using chemical oxidation enhanced chemical leaching, and aims at providing a repairing method of chemical oxidation enhanced chemical leaching adopted to increase removal rate of a leaching agent by eluting organic combined states of the heavy metals. The method comprises the following steps of (1) leaching with an oxidizing agent: performing vibration leaching on polluted soil by using an oxidizing agent solution, centrifuging and filtering to remove a leaching solution; and (2) leaching with a Na2EDTA aqueous solution: adding the Na2EDTA aqueous solution in the polluted soil leached by the oxidizing agent to carry out the vibration leaching, centrifuging and filtering to remove the leaching solution.
Description
Technical field
The present invention relates to heavy metal pollution of soil and administer the heavy metal adsorbed with the obligate that chemical bond form is combined with the soil organism in reparation field, particularly wash-out, the method for the chemical oxidation adopted strengthening chemical leaching.
Background technology
Along with the event such as " cadmium rice ", " blood lead " takes place frequently, heavy metal pollution of soil harmfulness all the more cause extensive attention, heavy metal pollution of soil administer extremely urgent, the research thus about heavy metal soil remediation receives much concern.Wherein, the parent that the reparation of biological prosthetic particularly over-accumulated plant obtains domestic and international expert with its low cost, environmental protection looks at, but because its growth cycle is long, it is slow to take effect, contaminated concentration, climatic effect is large and super enriching plant kind is less, screening process is slow, and thus its application is extremely restricted; Though the investment of solidification and stabilization technology is less, there is potential ecological risk owing to heavy metal can not be separated from soil, thus its application is also subject to larger restriction.Elution technique preferably resolves these problems, and it both can realize heavy metal and be separated from soil, has again the advantage of instant effect, not restricted climatic effect; The key of elution technique is the selection of eluent, and eluent has varied: inorganic eluent, artificial chelating agent, surfactant, organic acid etc., different eluent difference on effect is very big.Current, at home and abroad some heavy metal pollution of soil are administered in case and are employed elution technique, but poor effect, reason is except being limited by cost, the soil texture, pollution type, and the removal efficiency of eluent itself not high is also a very key factor; With Na in existing eluent
2the chemical leaching effect that EDTA carries out is the most obvious, but is subject to the impact of the soil texture and pollution type, and still can not be up to state standards far away value in the engineer applied of much reality.
According to the continuous extraction that Tessier proposes, effect of fertilizer generally can be divided into water-soluble state, exchange state, carbonate in conjunction with state, Fe-Mn oxide, combination state and residual in soil in occurrence patterns; Europe now adopts BCR extraction method, and the form of heavy metal is divided into 4 kinds of i.e. acid-soluble state, reducible state, oxidable state and residual forms by this method.It is variant according to soil types (as soil property, heavy metal kind) difference that soil morphology composes storage, for most of soil, heavy metal residual form proportion is maximum, but because of form stable, not easily extract and little to environmental perturbation, the research of this form is less; Except residual form, at all the other in several occurrence patterns, be more relatively not easily leached agent wash-out to organically combine state (or oxidable state).Find through large quantity research, proportion generally can about 10% in polluted agricultural land to organically combine state (or oxidable state) heavy metal in soil, during as research Xiaoqing River, Shandong Province irrigating region Heavy Metal Pattern in Soils such as Du Xiaolin, eight kinds of elements such as Cd, Zn, Pb, Cu, Cr are analyzed, wherein the oxidable state proportion of these five kinds of elements is respectively: 9.44%, 11.54%, 7.37%, 12.24%, 8.53%; Bend into and wait people to acquire Chaoyang, Beijing, Haidian District and Suburb Soil to having carried out the analysis of heavy metal occurrence patterns, wherein Zn organically combines state proportion between 5.3%-26.8%, and Pb is between 0-13.4%; Wang Qifeng shows ten, Guangdong vegetable field soil heavy metal Pb, Cd fractionation result of study, and shared by the oxidable state of Pb, Cd, average percent is 10.01%, 7.26%; And in some diggings barren site, oxidable state proportion can reach higher level, and Zhu Jiawen finds in Huayuan, western Hunan Pb-Zn ore district heavy-metal contaminated soil research bare area: Pb, Zn, Cd oxidation state proportion is respectively up to 43.82%, 22.19%, 32.82%.In a word, this form content is relatively large, and is difficult to wash-out, and thus improving this occurrence patterns has very significance to drip washing, and the present invention is just based on the research that this carries out.
Summary of the invention
In soil remediation, chemical oxidizing agent is generally applied to organic pollutant degradation; And in heavy-metal contaminated soil research, the research for washed off soil heavy metal has no report.The present invention focuses on research eluent and technique, changes medicament kind and consumption, using oxidating chemicals Fenton reagent solution as a kind of Soil leaching agent, and the auxiliary high-quality eluent Na through screening
2eDTA (disodium ethylene diamine tetraacetate).The process that the chemical oxidation adding heavy metal-polluted soil extracts, improves heavy metal-polluted soil meltage after drip washing, with the effect of backfill up to standard after reaching drip washing.
The problem that this restorative procedure is intended to solve that traditional ELUTION METHOD is not high to part heavy metal element soil elution rate, can not be up to standard after drip washing, by the heavy metal that wash-out adsorbs with the obligate that chemical bond form is combined with the soil organism, and the method combined with eluent.
For reaching above repairing effect, the present invention is the method for a kind of chemical oxidation strengthening chemical leaching restoration of soil polluted by heavy metal, comprises the following steps:
Aqueous oxidizing agent solution drip washing: use aqueous oxidizing agent solution to carry out concussion drip washing, centrifugal rear filtering leacheate to contaminated soil;
Na
2eDTA aqueous solution drip washing: add Na by the described contaminated soil after described aqueous oxidizing agent solution drip washing
2the EDTA aqueous solution carries out vibration drip washing, centrifugal rear filtering leacheate.
Wherein said Na
2also comprise after the drip washing of the EDTA aqueous solution and add the step that clear water carries out vibration drip washing, centrifugal rear filtering leacheate.
The compound concentration of the wherein said Fenton reagent aqueous solution is, FeSO
47H
2o dosage is 24g/L, H
2o
2(30%) dosage is 200ml/L, and pH is adjusted to 3-4.
Wherein said aqueous oxidizing agent solution and described contaminated soil liquid-solid ratio scope between 5:1 to 15:1, preferred 10:1; Described Na
2the EDTA aqueous solution and described contaminated soil liquid-solid ratio scope between 5:1 to 15:1, preferred 10:1.
Solution 0.1mol/L C in wherein said aqueous oxidizing agent solution rinsing step
6h
8o
7tune pH is 3-4, is preferably 3.
Wherein said Na
2in EDTA aqueous solution rinsing step, solution 0.1mol/L HCl or 0.1mol/LNaOH solution adjust pH to be between 3.9-8, and preferably 4.5.
The wherein said aqueous oxidizing agent solution drip washing time is 0.5-2 hour, preferably 1 hour; Described Na
2the EDTA aqueous solution drip washing time is 0.5-2 hour, preferably 1 hour.
By technique scheme, the present invention at least has following technique effect:
1, the heavy metal Main Morphology that existing eluent is removed concentrates on easy solvent and exchange state, and to being difficult to, eluted combination state removal effect is poor, often causes clearance not high; Use oxidant and the drip washing of eluent substep, improve heavy metal-polluted soil elution efficiency further, reduce ecological risk.
2, after drip washing, Iron in Soil oxide greatly reduces the activity of residual heavy metal in soil, forces heavy metal to be stablized further in soil.This is mainly owing to can cause the generation of new unformed or microstructure, a large amount of adsorbing metal ions or ion cluster when oxide new in lessivation generates; Ferriferous oxide generation Forms Transformation, heavy metal and its may occur to precipitate and co-precipitation, finally cause non-wash-out heavy metal activity in soil greatly to reduce.
Detailed description of the invention
Below in conjunction with embodiment, by carrying out drip washing to three kinds of different heavy metal concentration Polluted Soils, to above-mentioned being described in more detail with other technical characteristic and advantage of the present invention.
Embodiment 1
Gather mining area, somewhere 1 Soil Surrounding, survey its basic physical and chemical: cadmium: 1.34mg/kg, plumbous: 383mg/kg, zinc: 313mg/kg, pH=6.1, at room temperature carries out air-dry by adopted soil, and sieves particle diameter soil between 60 order-200 orders, stirs;
(1) take 10g soil and put into 250ml triangular flask, add 50ml0.5mol/L Na
2the EDTA aqueous solution, regulate pH to 4 with 0.1mol/L HCl, vibrate 50min under the horizontal hunting speed of room temperature is 200rpm, centrifugal, isolates soil and leacheate;
(2) the 0.5mol/L Na of 50ml is added again
2the EDTA aqueous solution, regulate pH to 4 with 0.1mol/L HCl, vibrate 50min under the horizontal hunting speed of room temperature is 200rpm, centrifugal, isolates soil and leacheate;
(3) by the soil after again centrifugal, add the deionized water of 50ml, vibrate 1h under the horizontal hunting speed of room temperature is 200rpm, centrifugal, isolates soil and leacheate.
Embodiment 2
Gather mining area, somewhere 1 Soil Surrounding, survey its basic physical and chemical: cadmium: 1.34mg/kg, plumbous: 383mg/kg, zinc: 313mg/kg, pH=6.1, at room temperature carries out air-dry by adopted soil, and sieves particle diameter soil between 60 order-200 orders, stirs;
(1) take 10g soil and put into 250ml triangular flask, (compound concentration is 24g/L FeSO to add the 50ml Fenton reagent aqueous solution
47H
2o, 200ml/L H
2o
2, use 0.1mol/L C
6h
8o
7regulate pH to 3), vibrate 50min under the horizontal hunting speed of room temperature is 200rpm, centrifugal, isolates soil and leacheate;
(2) soil after centrifugal, adds 50ml0.5mol/L Na
2the EDTA aqueous solution, regulate pH to 4 with 0.1mol/L HCl, vibrate 50min under the horizontal hunting speed of room temperature is 200rpm, centrifugal, isolates soil and leacheate;
(3) by the soil after again centrifugal, add the deionized water of 50ml, vibrate 1h under the horizontal hunting speed of room temperature is 200rpm, centrifugal, isolates soil and leacheate.
Embodiment 1 and 2 liang of group samples are after above Step gragient elution, and after measured, Cd, Pb, Zn content in soil increased in embodiment 2 after oxidation drip washing is respectively 0.45mg/kg, 217mg/kg, 178mg/kg.Only Na is used relative in example 1
2after the drip washing of the EDTA aqueous solution, heavy metal content in soil value 0.61mg/kg, 266mg/kg, 210mg/kg, improve 12.1%, 22.8% and 10.2% respectively, and clearance reaches 66.4%, 53.5% and 32.9%.After drip washing, heavy metal-polluted soil Pb, Zn content all reaches standard of soil environment quality value secondary standard, and Cd reaches standard of soil environment quality value grade III Standard.
Embodiment 3
Gather mining area, somewhere 1 Soil Surrounding, survey its basic physical and chemical: cadmium: 1.34mg/kg, plumbous: 383mg/kg, zinc: 313mg/kg, pH=6.1, at room temperature carries out air-dry by adopted soil, and sieves particle diameter soil between 60 order-200 orders, stirs;
(1) take 10g soil and put into 250ml triangular flask, add 100ml0.5mol/L Na
2the EDTA aqueous solution, regulate pH to 5 with 0.1mol/L HCl, vibrate 1h under the horizontal hunting speed of room temperature is 200rpm, centrifugal, isolates soil and leacheate;
(2) the 0.5mol/L Na of 100ml is added again
2the EDTA aqueous solution, regulate pH to 5 with 0.1mol/L HCl, vibrate 1h under the horizontal hunting speed of room temperature is 200rpm, centrifugal, isolates soil and leacheate;
(3) by the soil after again centrifugal, add the deionized water of 100ml, vibrate 1h under the horizontal hunting speed of room temperature is 200rpm, centrifugal, isolates soil and leacheate.
Embodiment 4
Gather mining area, somewhere 1 Soil Surrounding, survey its basic physical and chemical: cadmium: 1.34mg/kg, plumbous: 383mg/kg, zinc: 313mg/kg, pH=6.1, at room temperature carries out air-dry by adopted soil, and sieves particle diameter soil between 60 order-200 orders, stirs;
(1) take 10g soil and put into 250ml triangular flask, (compound concentration is 24g/L FeSO to add the 100ml Fenton reagent aqueous solution
47H
2o, 200ml/L H
2o
2, use 0.1mol/L C
6h
8o
7regulate pH to 3.5), vibrate 1h under the horizontal hunting speed of room temperature is 200rpm, centrifugal, isolates soil and leacheate;
(2) soil after centrifugal, adds 100ml0.5mol/L Na
2the EDTA aqueous solution, regulate pH to 5 with 0.1mol/LHCl, vibrate 1h under the horizontal hunting speed of room temperature is 200rpm, centrifugal, isolates soil and leacheate;
(3) by the soil after again centrifugal, add the deionized water of 100ml, vibrate 1h under the horizontal hunting speed of room temperature is 200rpm, centrifugal, isolates soil and leacheate.
Embodiment 3 and 4 liang of group samples are after above Step gragient elution, and after measured, Cd, Pb, Zn content in soil increased in embodiment 4 after oxidation drip washing is respectively 0.37mg/kg, 181mg/kg, 166mg/kg.Only Na is used relative in example 3
2after the drip washing of the EDTA aqueous solution, heavy metal content in soil value 0.54mg/kg, 250mg/kg, 201mg/kg, improve 12.7%, 18.0% and 11.2% respectively, and clearance reaches 72.4%, 52.7% and 47.0%.After drip washing, heavy metal-polluted soil Pb, Zn content all reaches standard of soil environment quality value secondary standard, and Cd reaches standard of soil environment quality value grade III Standard.
Embodiment 5
Gather certain severe mining area 2 contaminated soil, survey its basic physical and chemical: cadmium: 4.19mg/kg, plumbous: 761mg/kg, zinc: 493mg/kg, pH=7.06, at room temperature carries out air-dry by adopted soil, and sieve particle diameter soil between 60 order-200 orders, stir;
(1) take 10g soil and put into 250ml triangular flask, add the 0.5mol/L Na of 150ml
2the EDTA aqueous solution, regulate pH to 6.5 with 0.1mol/L HCl, vibrate 2h under the horizontal hunting speed of room temperature is 200rpm, centrifugal, isolates soil and leacheate;
(2) the 0.5mol/L Na of 150ml is added again
2the EDTA aqueous solution, regulate pH to 6.5 with 0.1mol/L HCl, vibrate 2h under the horizontal hunting speed of room temperature is 200rpm, centrifugal, isolates soil and leacheate;
(3) by the soil after again centrifugal, add the deionized water of 150ml, vibrate 1h under the horizontal hunting speed of room temperature is 200rpm, centrifugal, isolates soil and leacheate.
Embodiment 6
Gather certain severe mining area 2 contaminated soil, survey its basic physical and chemical: cadmium: 4.19mg/kg, plumbous: 761mg/kg, zinc: 493mg/kg, pH=7.06, at room temperature carries out air-dry by adopted soil, and sieve particle diameter soil between 60 order-200 orders, stir;
(1) take 10g soil and put into 250ml triangular flask, (compound concentration is 24g/L FeSO to add the 150ml certain concentration Fenton reagent aqueous solution
47H
2o, 200ml/L H
2o
2, use 0.1mol/L C
6h
8o
7solution regulates pH to 4), vibrate 2h under the horizontal hunting speed of room temperature is 200rpm, centrifugal, isolates soil and leacheate;
(2) soil after centrifugal, adds 150ml0.5mol/L Na
2the EDTA aqueous solution, regulate pH to 6.5 with 0.1mol/L HCl, vibrate 2h under the horizontal hunting speed of room temperature is 200rpm, centrifugal, isolates soil and leacheate;
(3) by the soil after again centrifugal, add the deionized water of 150ml, vibrate 1h under the horizontal hunting speed of room temperature is 200rpm, centrifugal, isolates soil and leacheate.
Embodiment 5 and embodiment 6 liang group sample are after above Step gragient elution, and after measured, the relative embodiment 6 of Cd, Pb, Zn clearance after embodiment 5 increases oxidation drip washing only uses Na
2eDTA aqueous solution drip washing clearance adds 4.93%, 9.05%, 12.5%, and after drip washing oxidation, the clearance of Cd, Pb, Zn concentration reaches 76.6%, 89.4%, 80.2% respectively.After drip washing, Pb, Zn are all up to state standards standard of soil environment quality value secondary standard, and Cd reaches grade III Standard.In embodiment 1-2,3-4 and 5-6, described eluent all achieves good drip washing effect under adopting the condition such as different pH, duration of oscillation, solid-to-liquid ratio within right.
How many according to soil in contaminated soil lessivation, type and drip washing quality requirement can suitably adjust aqueous oxidizing agent solution solution concentration, Na
2pH value of solution in EDTA concentration of aqueous solution, leacheate and contaminated soil liquid-solid ratio, each rinsing step, the drip washing time etc., to realize optimum repairing effect.
Above-described embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that those of ordinary skill in the art make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determines.
Claims (9)
1. a method for chemical oxidation strengthening chemical leaching restoration of soil polluted by heavy metal, is characterized in that comprising following steps:
Aqueous oxidizing agent solution drip washing: use aqueous oxidizing agent solution to carry out concussion drip washing, centrifugal rear filtering leacheate to contaminated soil;
Na
2eDTA aqueous solution drip washing: add Na by the described contaminated soil after described aqueous oxidizing agent solution drip washing
2the EDTA aqueous solution carries out vibration drip washing, centrifugal rear filtering leacheate.
2. the method for chemical oxidation strengthening chemical leaching restoration of soil polluted by heavy metal as claimed in claim 1, is characterized in that: described Na
2also comprise after the drip washing of the EDTA aqueous solution and add the step that clear water carries out vibration drip washing, centrifugal rear filtering leacheate.
3. the method for chemical oxidation strengthening chemical leaching restoration of soil polluted by heavy metal as claimed in claim 1, is characterized in that: described aqueous oxidizing agent solution is Fenton reagent solution.
4. the method for chemical oxidation strengthening chemical leaching restoration of soil polluted by heavy metal as claimed in claim 3, is characterized in that: described Fenton reagent solution preparation concentration is FeSO
47H
2o dosage is 24g/L, H
2o
2(30%) dosage is 200ml/L, and pH is adjusted to 3-4.
5. the method for chemical oxidation strengthening chemical leaching restoration of soil polluted by heavy metal as claimed in claim 1, is characterized in that: described Na
2eDTA concentration of aqueous solution is 0.1-1mol/L, preferred 0.5mol/L.
6. the method for chemical oxidation strengthening chemical leaching restoration of soil polluted by heavy metal as claimed in claim 1, is characterized in that: described aqueous oxidizing agent solution and described contaminated soil liquid-solid ratio scope between 5:1 to 15:1, preferred 10:1; Described Na
2the EDTA aqueous solution and described contaminated soil liquid-solid ratio scope between 5:1 to 15:1, preferred 10:1.
7. the method for chemical oxidation strengthening chemical leaching restoration of soil polluted by heavy metal as claimed in claim 1, is characterized in that: described aqueous oxidizing agent solution pH 0.1mol/L C
6h
8o
7be adjusted to 3-4, preferred pH is 3.
8. the method for chemical oxidation strengthening chemical leaching restoration of soil polluted by heavy metal as claimed in claim 1, is characterized in that: described Na
2in EDTA aqueous solution rinsing step, the NaOH of pH value of solution 0.1mol/L HCl or 0.1mol/L is adjusted to 3.9-8, and preferred pH is 4.5.
9. the method for chemical oxidation strengthening chemical leaching restoration of soil polluted by heavy metal as claimed in claim 1, is characterized in that: the described aqueous oxidizing agent solution drip washing time is 0.5-2 hour, preferably 1 hour; Described Na
2the EDTA aqueous solution drip washing time is 0.5-2 hour, preferably 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 |
| CN111672898A (en) * | 2020-06-30 | 2020-09-18 | 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 |
| CN114275984A (en) * | 2021-12-22 | 2022-04-05 | 华中科技大学 | Electrochemical leaching lead recovery method for lead-containing sludge |
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Cited By (8)
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|---|---|---|---|---|
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| 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 |
| CN111672898A (en) * | 2020-06-30 | 2020-09-18 | 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 |
| CN114275984A (en) * | 2021-12-22 | 2022-04-05 | 华中科技大学 | Electrochemical leaching lead recovery method for lead-containing sludge |
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