CN106825013A - Using the method for modified Nano Zero-valent Iron heavy metal contaminated soil stabilization processes - Google Patents
Using the method for modified Nano Zero-valent Iron heavy metal contaminated soil stabilization processes Download PDFInfo
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- CN106825013A CN106825013A CN201710106612.2A CN201710106612A CN106825013A CN 106825013 A CN106825013 A CN 106825013A CN 201710106612 A CN201710106612 A CN 201710106612A CN 106825013 A CN106825013 A CN 106825013A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
- B09C1/08—Reclamation of contaminated soil chemically
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Abstract
Field is repaired the invention belongs to pollute Heavy Metals In Environment, a kind of method of the stabilization processes of utilization modified Nano Zero-valent Iron heavy metal contaminated soil is disclosed, it is comprised the following steps：（1）The pre-treatment of soil；（2）The preparation of modified Nano Zero-valent Iron；（3）Modified Nano Zero-valent Iron mixes with soil；（4）Modified Nano Zero-valent Iron stabilizes heavy-metal composite pollution soil assessment.It is characteristic of the invention that being modified to nano zero valence iron using polyvinylpyrrolidone, acted on by steric hindrance and electrostatic steric effect, reduce the reunion of nano zero valence iron, increase its dispersiveness and the animal migration in soil, after measured using the present invention, modified nano zero valence iron dispersiveness and animal migration increase in soil, it is not easy to adsorbed by solid phase of soil, in 1h, only 19.7% P nZVI are by adsorption by soil.
Description
Technical field
Field is repaired the invention belongs to pollute Heavy Metals In Environment, more particularly to it is a kind of using modified Nano Zero-valent Iron
The method of the stabilization processes of heavy metal contaminated soil.
Background technology
The administration of mankind's activity such as mining, metal smelt, Wastewater Irrigation in Farmland, agricultural sludge and fertilizer and insecticide,
Substantial amounts of heavy metal pollution of soil has been had resulted in, the ecological balance, food security and health has seriously been threaten.Wherein cadmium
（Cd）, mercury（Hg）, arsenic（As）, chromium（Cr）And lead（Pb）It is considered as " five poisonous creatures: scorpion, viper, centipede, house lizard, toad " in Main Heavy Metal.《National soil
Survey of contaminating status publication》Middle display：The total exceeding standard rate of national soil is 16.1%, and pollution type is inorganic based on inorganic type
Exceeded digit of pollutant accounts for the 82.8% of all super punctuation bits, and arable soil point position exceeding standard rate is 19.4%.Mining and metallurgy activity is weight
The main source of metallic pollution.It is either relatively light by the abandoned location of industry and mining that heavy metal pollution is more serious, or pollution level
Agricultural pollution soil, often show as the combined pollution of various heavy.It is increasingly complex, a various huge sum of moneys for contaminated soil
Reciprocation would generally occur between category, be that heavy metal pollution of soil is administered and the application of recovery technique brings difficulty.
The non-biodegradable of heavy metal determines it by long-term existence in soil.In order to reduce the life of heavy metal contaminants
Thing validity and animal migration, in numerous Heavy Metal Pollution Control technologies, the stabilization technology of heavy metal is considered as economical
Effectively and to the less recovery technique of environmental perturbation, increasingly it is taken seriously, and is gradually applied to repairing for heavy metal pollution place
It is multiple.Zero-valent Iron（Zero valent iron, ZVI）Technology, because its operating procedure is simple, treatment effeciency is high, operating cost is low, energy
The features such as small, material of consumption is easy to get, is considered as a kind of more potential soil stabilization recovery technique.Wherein, the zeroth order of Nano grade
Iron（Nano-scale zero-valent iron, nZVI）With going back that common grade or micron order Zero-valent Iron can not compare
Former adsorption capacity, efficient can must be changed into low toxicity or inertia by pollutant, such as chlorinated organics, toxic metals, inorganic compound
Material, applied in water environment, but still lack research and application in soil.
Due to nano zero valence iron particle surface electrostatic charge gravitation, high surface energy, intergranular Van der Waals force and particle
The hydrogen bond on surface and other chemical bonds, cause nano particle easily to form condensate, and nano zero valence iron Zero-valent Iron easily quilt
Oxidation, the two defects constrain its dispersiveness, animal migration in polluted-water and soil, are to limit its repair ability most
Big obstacle.Therefore, nano zero valence iron is modified, and is applied to combined pollution heavy metal soil, heavy metal combined pollution
The reparation of soil is significant.
The content of the invention
In order to solve the above technical problems, simple to operate it is an object of the invention to provide one kind, remediation efficiency is high, repairs into
This is low, and avoids causing environment the nano zero valence iron of the utilization polyvinyl pyrrolidone modified of secondary pollution in Compound Heavy Metals
The stabilization treatment method of contaminated soil.
To realize above-mentioned technical purpose, the present invention uses following technical scheme：
A kind of method of the stabilization processes of utilization modified Nano Zero-valent Iron heavy metal contaminated soil, it is characterised in that described
Method is comprised the following steps：Step（1）Soil pre-treatment, step（2）Prepared by modified Nano Zero-valent Iron, step（3）Modified Nano
Zero-valent Iron mixes with soil, step（4）Modified Nano Zero-valent Iron stabilizes heavy-metal composite pollution soil assessment.
Specifically, the described method comprises the following steps：
Step（1）Soil pre-treatment：By heavy-metal contaminated soil be placed on well-ventilated, it is clean and tidy, dustless, without effumability chemicals
The room of matter is air-dried, and the heavy-metal contaminated soil after air-drying is ground, and crosses 2mm nylon mesh, completes the pretreatment of soil；
Step（2）It is prepared by modified Nano Zero-valent Iron：It is the FeSO of 0.01M toward concentration under room temperature, nitrogen protection4Add in solution
Enter polyvinylpyrrolidone（PVP K-30）, mechanical agitation is allowed to be sufficiently mixed, and incorporation time is 15min, is subsequently adding concentration
It is the NaBH of 0.03M4Solution, under nitrogen protective condition, mechanical agitation, incorporation time 20min is obtained modified Nano Zero-valent Iron
Particle；Vacuum filtration after standing five minutes, washing；
Step（3）Modified Nano Zero-valent Iron mixes with soil：By step（2）In obtain modified Nano zero-valent iron particle, add
Ultra-pure water, is quickly stirred with mechanical agitator, is made modified Nano zeroth order ferrous solution, then adds modified Nano zeroth order ferrous solution
Enter to step（1）In the middle soil by pre-treatment, and make soil moisture saturation with water, vibrated with constant temperature oscillation machine, then exist
Ventilation condition preferably interior standing, carries out stabilization processes；
Step（4）Modified Nano Zero-valent Iron stabilizes heavy-metal composite pollution soil assessment：To step（3）Middle Fe0 In soil
Stability is measured.
The step（1）In, the pH of the heavy-metal contaminated soil is 7.4.
The step（3）In, the concentration of the modified Nano zeroth order ferrous solution is 1.0g/L.
The step（2）In, the churned mechanically speed is 300rpm.
The step（3）In, the constant temperature oscillation machine parameter of oscillation is：Vibration more than 10h, temperature is 20 DEG C~30 DEG C,
Rotating speed is 150rpm.
The step（3）In, indoor time of repose is 14 days~21 days.
Compared with prior art, advantages of the present invention mainly includes but is not limited to the following aspects：
New modified nano zero valence iron prepared by the present invention can be used to administer heavy-metal composite pollution soil, and its is easy to operate, behaviour
Make simple, remediation efficiency is high, and rehabilitation cost is low, and avoids causing environment secondary pollution, therefore has in environment remediation field
It is widely applied prospect.
The present invention is modified as stabilizer using polyvinylpyrrolidone to nano zero valence iron, the modified Nano zero for obtaining
Valency iron is a kind of good with dispersive property, and stability and animal migration are good in soil, remediation efficiency material high.
In the preparation method of the modified Nano Zero-valent Iron that the present invention is used, by BH4 -/Fe2+Mol ratio be 3.0 proportioning
Under the conditions of be prepared, make Fe2+Restore All is into Fe0, reaction efficiency is high；Secondly, the reagent and equipment for being used easily are obtained,
Prepare easy；Finally, reacted product is modified nano zero-valence iron particle precipitation, it is easy to separated from solution, can be most
Purity modified Nano Zero-valent Iron higher is obtained eventually.Compared to other method, modified Nano Zero-valent Iron dispersion prepared by the present invention
Property it is strong, be difficult to reunite, the stability and animal migration in soil are stronger, can effectively Compound Heavy Metals in stable soil.
Heavy metal combined contamination soil of the present invention carries out stabilisation reparation, and remediation efficiency is high, and operation is simple, repairs
Low cost, in can be applied to large-scale heavy-metal composite pollution soil.
Brief description of the drawings
Fig. 1 is the transmission electron microscope picture of unmodified nano zero valence iron
Fig. 2 is the transmission electron microscope picture of the nano zero valence iron of polyvinyl pyrrolidone modified
Fig. 3 is curve of adsorption kinetics of the soil to nZVI and P-nZVI.
Specific embodiment
In order that those skilled in the art more fully understand the technical scheme in the application, below in conjunction with the application tool
Body embodiment, is more clearly and completely described to the present invention, it is clear that described embodiment is only the application one
Divide embodiment, rather than whole embodiments.Based on the embodiment in the application, those of ordinary skill in the art are not making
The every other embodiment obtained under the premise of creative work, should all belong to the scope of protection of the invention.
Embodiment 1
Heavy-metal composite pollution soil is pre-processed
（1）Heavy-metal composite pollution soil is placed on well-ventilated, room wind clean and tidy, dustless, without effumability chemical substance
It is dry；
（2）Heavy-metal composite pollution soil after air-drying, is ground with mallet, wood rolling and poly (methyl methacrylate) plate, crosses 2mm nylon
Sieve, completes the pretreatment of soil.
Prepare modified Nano Zero-valent Iron：
（1）FeSO4The preparation of solution：Weigh 0.1400gFeSO4·7H2O is placed in beaker, adds appropriate ultra-pure water, uses glass
Rod stirring and dissolving, and be transferred in 50ml volumetric flasks, graduation mark is settled to, shake up, as 0.01M FeSO4Solution.
（2）FeSO containing polyvinylpyrrolidone4The preparation of solution：0.4g polyvinylpyrrolidones are weighed, in nitrogen
Under conditions of protection and agitator stirring, it is allowed to be dissolved in 50ml 0.01M FeSO4In solution, 15min is stirred.
（3）NaBH4The preparation of solution：Weigh 0.0567g NaBH4It is placed in beaker, adds appropriate ultra-pure water, uses glass bar
Stirring and dissolving, and be transferred in 50ml volumetric flasks, graduation mark is settled to, shake up, as 0.03M NaBH4Solution.
（4）Nano zero valence iron（nZVI）Preparation：At room temperature, by the FeSO of 50mL4Solution is placed in 250ml there-necked flasks
In, under conditions of nitrogen protection and agitator stirring, by the NaBH of 50mL4The rapid uniform speed slow of the aqueous solution drops to three mouthfuls of burnings
In bottle, continue to stir 20min, obtain black suspension.Vacuum filtration after standing five minutes, respectively with ultra-pure water and absolute ethyl alcohol
Washing 3 times, under nitrogen protection, 10h is dried in 40 DEG C of baking ovens, is dried.
（5）Modified Nano Zero-valent Iron（P-nZVI）Preparation：At room temperature, 50mL is contained into polyvinylpyrrolidone
FeSO4Solution is placed in 250ml there-necked flasks, under conditions of nitrogen protection and agitator stirring, by the NaBH of 50mL4It is water-soluble
The rapid uniform speed slow of liquid is dropped in there-necked flask, continues to stir 20min, obtains black suspension.Vacuum after standing five minutes
Suction filtration, respectively with ultra-pure water and absolute ethanol washing 3 times, under nitrogen protection, 10h is dried in 40 DEG C of baking ovens, is dried.
（6）Nano zero valence iron after drying（nZVI）With the nano zero valence iron of polyvinyl pyrrolidone modified（P-nZVI）Can
Be placed in glove box or 5% ethanol solution in preserve.
The nano zero valence iron of above-mentioned preparation（nZVI）With the nano zero valence iron of polyvinyl pyrrolidone modified（P-nZVI）Electricity
Sem observation result is shown in Fig. 1 and Fig. 2.
Embodiment 2
Investigate the nano zero valence iron of polyvinyl pyrrolidone modified（P-nZVI）Stability in heavy-metal composite pollution soil
Determine.
（1）Fe0The preparation of solution：Weigh the nano zero valence iron of certain mass（nZVI）, polyvinyl pyrrolidone modified
Nano zero valence iron iron（P-nZVI）Ultrasound 3min obtains nZVI solution N, P-nZVI solution in being each dissolved in the pure water of removal oxygen
Fe in P, N and P0Concentration is 1.0g/L.
（2）Respectively at addition 12g sieving heavy-metal composite pollution soil in 100mL centrifuge tubes, and add 63mL deionizations
Water, stands 14 days at room temperature.
（3）93% supernatant is replaced with the N of same volume, P（Fe=1.0g/L）, it is subsequently placed into shaking table vibration 70h.
When 1h, 5h, 10h, 20h, 40h, 60h, 400g centrifugation 10min separate free nano zero valence iron with soil, take 1mL supernatants
Liquid.
（4）1mL supernatants, the HCl for adding 4ml concentration to be 12 M is cleared up, and Fe contents are measured with ICP-MS, and
By being calculated the nZVI and P-nZVI that are adsorbed by solid phase of soil.
From figure 3, it can be seen that the nano zero valence iron iron of polyvinyl pyrrolidone modified（P-nZVI）It is more compound than in heavy metal
Stability in contaminated soil is far better than nano zero valence iron（nZVI）.Increase over time, add nano zero valence iron
（nZVI）, polyvinyl pyrrolidone modified nano zero valence iron iron（P-nZVI）Stabilization processes after, adsorbed by solid phase of soil
Fe contents constantly increase.Wherein nZVI, it is very fast to the rate of adsorption of Fe in initial 0-10h soil, over time
Increase, the rate of adsorption gradually slows down, and nZVI tends to be balanced in 40h, P- is far longer than by the amount that solid phase of soil is adsorbed during 60h
nZVI.P-nZVI is not easy to be adsorbed by solid phase of soil, and in 1h, only 19.7% P-nZVI is reached by adsorption by soil in 20h
To balance, adsorbed ratio is 74.1%, is 77.9% in 60h.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specific example " or
The description of " some examples " etc. means that combining the embodiment or specific features, structure, material or the feature of example description includes
In at least one embodiment of the invention or example.In this manual, to the schematic representation of above-mentioned term necessarily pin
To be identical embodiment or example.Although embodiments of the invention have been shown and described above, it is to be understood that
Above-described embodiment is exemplary, it is impossible to be interpreted as limitation of the present invention, one of ordinary skill in the art is of the invention
In the range of above-described embodiment can be changed, change, replace and modification.
Claims (7)
1. a kind of method of the stabilization processes of utilization modified Nano Zero-valent Iron heavy metal contaminated soil, it is characterised in that institute
The method of stating is comprised the following steps：Step（1）Soil pre-treatment, step（2）Prepared by modified Nano Zero-valent Iron, step（3）It is modified to receive
Rice Zero-valent Iron mixes with soil, step（4）Modified Nano Zero-valent Iron stabilizes heavy-metal composite pollution soil assessment.
2. method according to claim 1, it is characterised in that the described method comprises the following steps：
Step（1）Soil pre-treatment：By heavy-metal contaminated soil be placed on well-ventilated, it is clean and tidy, dustless, without effumability chemicals
The room of matter is air-dried, and the heavy-metal contaminated soil after air-drying is ground, and crosses 2mm nylon mesh, completes the pretreatment of soil；
Step（2）It is prepared by modified Nano Zero-valent Iron：It is the FeSO of 0.01M toward concentration under room temperature, nitrogen protection4Added in solution
Polyvinylpyrrolidone（PVP K-30）, mechanical agitation is allowed to be sufficiently mixed, and incorporation time is 15min, is subsequently adding concentration and is
The NaBH of 0.03M4Solution, under nitrogen protective condition, mechanical agitation, incorporation time 20min is obtained modified Nano Zero-valent Iron
Grain；Vacuum filtration after standing five minutes, washing；
Step（3）Modified Nano Zero-valent Iron mixes with soil：By step（2）In obtain modified Nano zero-valent iron particle, add
Ultra-pure water, is quickly stirred with mechanical agitator, is made modified Nano zeroth order ferrous solution, then adds modified Nano zeroth order ferrous solution
Enter to step（1）In the middle soil by pre-treatment, and make soil moisture saturation with water, vibrated with constant temperature oscillation machine, then exist
Ventilation condition preferably interior standing, carries out stabilization processes；
Step（4）Modified Nano Zero-valent Iron stabilizes heavy-metal composite pollution soil assessment：To step（3）Middle Fe0 In soil
Stability is measured.
3. method according to claim 2, it is characterised in that the step（1）In, the pH of the heavy-metal contaminated soil
It is 7.4.
4. method according to claim 2, it is characterised in that the step（3）In, the modified Nano zeroth order ferrous solution
Concentration be 1.0g/L.
5. method according to claim 2, it is characterised in that the step（2）In, the churned mechanically speed is
300rpm。
6. method according to claim 2, it is characterised in that the step（3）In, the constant temperature oscillation machine parameter of oscillation
For：Vibration more than 10h, temperature is 20 DEG C~30 DEG C, and rotating speed is 150rpm.
7. method according to claim 2, it is characterised in that the step（3）In, indoor time of repose is 14 days~21
My god.
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Cited By (9)
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| CN108246794A (en) * | 2018-03-01 | 2018-07-06 | 环境保护部南京环境科学研究所 | Improve method of the nano zero valence iron in heavy-metal composite pollution soil stabilization efficiency |
| CN108555010A (en) * | 2018-01-31 | 2018-09-21 | 中冶华天南京工程技术有限公司 | Application and method of the nano zero valence iron of Chitosan-coated in removal heavy-metal contaminated soil antimony |
| CN108787723A (en) * | 2018-06-19 | 2018-11-13 | 浙江省农业科学院 | The processing method and equipment of soil polluted by organic chloride reparation |
| CN109231782A (en) * | 2018-10-17 | 2019-01-18 | 桂林理工大学 | The minimizing stabilization treatment method of Cd in a kind of municipal sludge |
| CN109652080A (en) * | 2019-01-09 | 2019-04-19 | 中国农业大学 | A kind of soil-repairing agent and preparation method thereof |
| CN111633021A (en) * | 2020-06-08 | 2020-09-08 | 上海大学 | Nano zero-valent iron modified composite mesoporous material and preparation method and application thereof |
| CN112852436A (en) * | 2020-12-30 | 2021-05-28 | 苏州中科先进技术研究院有限公司 | Nano zero-valent iron-loaded porous polyimidazole nano-film and preparation method and application thereof |
| CN114832769A (en) * | 2022-05-17 | 2022-08-02 | 青岛科技大学 | Oxalate modified nano zero-valent iron material and preparation method and application thereof |
| CN115193426A (en) * | 2022-07-22 | 2022-10-18 | 中国环境科学研究院 | Modified nano zero-valent iron and preparation method and application thereof |
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| CN108555010A (en) * | 2018-01-31 | 2018-09-21 | 中冶华天南京工程技术有限公司 | Application and method of the nano zero valence iron of Chitosan-coated in removal heavy-metal contaminated soil antimony |
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| CN112852436A (en) * | 2020-12-30 | 2021-05-28 | 苏州中科先进技术研究院有限公司 | Nano zero-valent iron-loaded porous polyimidazole nano-film and preparation method and application thereof |
| CN112852436B (en) * | 2020-12-30 | 2023-09-19 | 苏州中科先进技术研究院有限公司 | Porous polyimidazole nano-film loaded with nano zero-valent iron, and preparation method and application thereof |
| CN114832769A (en) * | 2022-05-17 | 2022-08-02 | 青岛科技大学 | Oxalate modified nano zero-valent iron material and preparation method and application thereof |
| CN114832769B (en) * | 2022-05-17 | 2024-03-26 | 青岛科技大学 | Oxalate modified nano zero-valent iron material and preparation method and application thereof |
| CN115193426A (en) * | 2022-07-22 | 2022-10-18 | 中国环境科学研究院 | Modified nano zero-valent iron and preparation method and application thereof |
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