CN105945044A - Non-destructive repairing method for heavy metal contaminated soil - Google Patents
Non-destructive repairing method for heavy metal contaminated soil Download PDFInfo
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- CN105945044A CN105945044A CN201610315697.0A CN201610315697A CN105945044A CN 105945044 A CN105945044 A CN 105945044A CN 201610315697 A CN201610315697 A CN 201610315697A CN 105945044 A CN105945044 A CN 105945044A
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- soil
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- heavy metal
- carboxylic acid
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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
- B09C1/02—Extraction using liquids, e.g. washing, leaching, flotation
Abstract
The invention discloses a non-destructive repairing method for heavy metal contaminated soil. The method comprises the steps that to-be-treated soil is broken through a rotary cultivator; then, irrigation is conducted, and part of heavy metal fixed in soil is dissolved out; nanometer particles with Fe3O4 as a core and SiO2 as a shell are added into the soil to serve as adsorbent, and nitrogen containing macro-ring carboxylic acid derivate is modified on the edge of the shell of the particles of a core and shell structure; after adsorption treatment, the adsorbent adsorbing the heavy metal is separated out through an electromagnetic harrow device, a buffer solution and carbon microspheres are added in the separated-out soil, stirring and standing are conducted, and supernate is removed; and then, the soil is washed by purified water several times, and the treated soil is obtained. The soil treated through the method is free of secondary contamination, the heavy metal removing rate is high, efficiency is high, and cost is low.
Description
Technical field:
The present invention relates to contaminated soil process field, be specifically related to the lossless reparation side of a kind of heavy-metal contaminated soil
Method.
Background technology:
Along with China's industrialization, urbanization, the continuous quickening of the intensive process in rural area, heavy metal pollution of soil is asked
Topic becomes increasingly conspicuous.In urban environment, owing to industry and mankind's activity bring substantial amounts of heavy metal into urban soil
In, cause the accumulation in soil of these elements, and by air, water body or food chain directly or indirectly
Threaten the health of the mankind.Therefore, soil pollution reparation has become the vital task of field of Environment Protection.
It is dirty that Chinese patent (201110360190.4) discloses a kind of nano zero valence iron-electromagnetism rake remediating heavy metal
Dye soil/sludge processes, is to use Zero-valent Iron as adsorbent and to combine electromagnetism rake technology and effectively remove in soil
Heavy metal, although the method can effectively remove the heavy metal in soil, but its adsorbance is little, rehabilitating soil
Time adsorbent addition big, substantially increase the cost of soil remediation.
Summary of the invention:
It is an object of the invention to provide the lossless restorative procedure of a kind of heavy-metal contaminated soil, the method can be effective
Heavy metal is separated, and efficiency is high, low cost.
For achieving the above object, the present invention is by the following technical solutions:
The lossless restorative procedure of a kind of heavy-metal contaminated soil, comprises the following steps:
(1) by one block of dry soil by heavy metal pollution, crush with rotary cultivator, top layer 0.5-1m
Soil breaking reach 10-15cm to diameter less than the soil block of 3mm, the hydrops layer irrigated to soil horizon,
Stir 10-20h at 25-30 DEG C, make the part leaching ability of heavy metal being fixed in soil；
(2) soil after step (1) is irrigated adds Fe3O4For nuclear core, SiO2Nano-particle for shell
As adsorbent, the shell edge of this core-shell structure particles is modified with nitrogen heterocyclic ring carboxylic acid derivates, at 25-30 DEG C
Lower stirring 5-10h, then uses electromagnetism rake device to be separated by the adsorbent being adsorbed with heavy metal, and to dividing
Soil after from adds buffer, is simultaneously introduced carbosphere, mechanical agitation 20-40min, stands 10-15h,
Remove supernatant, 2-3 time the most repeatedly, finally use pure water soil 1-3 time, the soil after being governed.
Preferred as technique scheme, in step (2), the ring bone of described nitrogen heterocyclic ring carboxylic acid derivates
Containing atom N on frame, the atom N on ring skeleton is connected with carboxyl arm, and described carboxyl arm is positioned at outside ring.
Preferred as technique scheme, in step (2), described nitrogen heterocyclic ring carboxylic acid derivates is Isosorbide-5-Nitrae, 7-
7-triazacyclononane-1,4,7-triacetic acid, Cyclen-1,4,7,10-tetraacethyl,
1,4,8,11-tetraazacyclododecane tetradecane-1,4,8,11-tetraacethyl, 1,4,7,10,13-five-nitrogen heterocyclic pentadecane
-1,4,7,10,13-pentaacetic acid, 1,4,7,10,13,16-hexanitrogen heterocycle octadecane-1,4,7,10,13,16-six second
One in acid.
Preferred as technique scheme, in step (2), the preparation method of described adsorbent includes following
Step:
A nitrogen heterocyclic ring carboxylic acid derivates is dissolved in the biological buffer that pH is 5.3-5.5 by (), nitrogen is protected
Protect down, add catalyst EDC HCl and NHS, stir 1.5-3h under room temperature, obtain nitrogen heterocyclic ring carboxylic acid and spread out
Biological activated intermediate；
B () adds amino functional in the activated intermediate of the prepared nitrogen heterocyclic ring carboxylic acid derivates of step (a)
The magnetic microsphere changed, after ultrasonic disperse, reacts 8-10h at 25 ± 5 DEG C, and reaction separates with Magnet after terminating
Product, and replace cleaning product for several times with 0.1mol/L HCl solution, second alcohol and water, it is vacuum dried 10-20h,
Obtain adsorbent.
Preferred as technique scheme, in step (b), the magnetic microsphere of described amino functional be with
Fe3O4Magnetic nanoparticle is nuclear core, SiO2For protection shell, shell contains terminal amino group structure.
Preferred as technique scheme, in step (a), described nitrogen heterocyclic ring carboxylic acid derivates, EDC HCl,
The mol ratio of NHS is 1:(10-40): (5-15).
Preferred as technique scheme, in step (a), described biological buffer solutions is 1mol/L's
Quinoline ethyl sulfonic acid aqueous solution.
Preferred as technique scheme, in step (2), described buffer be concentration be 50-100mol/L
Bodied ferric sulfate and concentration be the oxalic acid solution of 0.3-0.5mol/L be the mixture of 1:1 according to volume ratio.
Preferred as technique scheme, in step (2), the buffer of described addition and the body of carbosphere
Long-pending ratio is (10-15): 1.
The method have the advantages that
Magnetic adsorbent prepared by the present invention, by the amidation process of EDC HCl, NHS catalysis, by azepine
Macro ring carboxylic acid derivates modifies the SiO of magnetic composite microsphere2Shell edge, its excellent adsorption, can effectively remove
Heavy metal ion in electroplating effluent, technique power consumption is low, can realize large-scale production, and its suction capacity is big, suction
Attached speed is fast, and the total removal rate of heavy metal ion reaches more than 98%；
The present invention uses Fe3O4Magnetic nanoparticle is nuclear core, SiO2For protection shell, shell contains end ammonia
The nano-particle of based structures is as adsorbent, and combines running vehicle type electromagnetism rake technology, effectively removes contaminated soil
In heavy metal, efficiency is high, and processing cost is low, to soil non-secondary pollution.
Detailed description of the invention:
In order to be better understood from the present invention, below by embodiment, the present invention is further described, and embodiment is only used
In explaining the present invention, the present invention will not be constituted any restriction.
Embodiment 1
The lossless restorative procedure of a kind of heavy-metal contaminated soil, comprises the following steps:
(1) preparation of adsorbent:
A 1mol 1,4,7-7-triazacyclononane-1,4,7-triacetic acid is dissolved in the life that pH is 5.3-5.5 by ()
In thing buffer, under nitrogen protection, add 10mol catalyst EDC HCl and 5molNHS, stir under room temperature
1.5h, obtains the activated intermediate of nitrogen heterocyclic ring carboxylic acid derivates；
B () adds Fe in the activated intermediate of the prepared nitrogen heterocyclic ring carboxylic acid derivates of step (a)3O4Magnetic
Property nano-particle is nuclear core, SiO2For protection shell, shell contains the nano-particle of terminal amino group structure, super
After sound dispersion, at 25 ± 5 DEG C, react 8h, reaction terminate after with Magnet separation product, and use 0.1mol/L HCl
Solution, second alcohol and water replace cleaning product for several times, are vacuum dried 10h, obtain adsorbent；
(2) by one block of dry soil by heavy metal pollution, crush with rotary cultivator, top layer 0.5m's
Soil breaking is less than the soil block of 3mm to diameter, and the hydrops layer irrigated to soil horizon reaches 10m, at 25-30 DEG C
Lower stirring 10h, makes the part leaching ability of heavy metal being fixed in soil；
(3) soil after step (2) is irrigated adds the adsorbent that step (1) prepares, at 25-30 DEG C
Lower stirring 5h, then uses electromagnetism rake device to be separated by the adsorbent being adsorbed with heavy metal, and after separating
Soil in add the bodied ferric sulfate of 50mol/L with concentration be the oxalic acid solution of 0.3mol/L, both add
Entering amount is that every 40kg soil is separately added into 2kg, 4kg, is simultaneously introduced 0.5kg carbosphere, mechanical agitation 20min,
Stand 10h, remove supernatant, 2-3 time the most repeatedly, finally use pure water soil 1-3 time, controlled
Soil after reason.
Embodiment 2
(1) preparation of adsorbent:
A () is by molten for 1mol 1,4,7,10,13,16-hexanitrogen heterocycle octadecane-1,4,7,10,13,16-six acetic acid
Solution, in the biological buffer that pH is 5.3-5.5, under nitrogen protection, adds 40mol catalyst EDC HCl
And 15molNHS, stir 3h under room temperature, obtain the activated intermediate of nitrogen heterocyclic ring carboxylic acid derivates；
B () adds Fe in the activated intermediate of the prepared nitrogen heterocyclic ring carboxylic acid derivates of step (a)3O4Magnetic
Property nano-particle is nuclear core, SiO2For protection shell, shell contains the nano-particle of terminal amino group structure, super
After sound dispersion, at 25 ± 5 DEG C, react 10h, reaction terminate after with Magnet separation product, and use 0.1mol/L HCl
Solution, second alcohol and water replace cleaning product for several times, are vacuum dried 20h, obtain adsorbent；
(2) by one block of dry soil by heavy metal pollution, crush with rotary cultivator, the soil of top layer 1m
Earth is crushed to the diameter soil block less than 3mm, and the hydrops layer irrigated to soil horizon reaches 15cm, at 25-30 DEG C
Stirring 20h, makes the part leaching ability of heavy metal being fixed in soil；
(3) soil after step (2) is irrigated adds the adsorbent that step (1) prepares, at 25-30 DEG C
Lower stirring 10h, then uses electromagnetism rake device to be separated by the adsorbent being adsorbed with heavy metal, and to separation
After soil in add the bodied ferric sulfate of 100mol/L with concentration be the oxalic acid solution of 0.5mol/L, both
Addition is that every 50kg soil is separately added into 5kg, 5kg, is simultaneously introduced 1kg carbosphere, mechanical agitation 40min,
Stand 15h, remove supernatant, 2-3 time the most repeatedly, finally use pure water soil 1-3 time, controlled
Soil after reason.
Embodiment 3
(1) preparation of adsorbent:
A 1mol Cyclen-1,4,7,10-tetraacethyl is dissolved in pH by ()
In the biological buffer of 5.3-5.5, under nitrogen protection, add 20mol catalyst EDC HCl and 7molNHS,
Stir 1.8h under room temperature, obtain the activated intermediate of nitrogen heterocyclic ring carboxylic acid derivates；
B () adds Fe in the activated intermediate of the prepared nitrogen heterocyclic ring carboxylic acid derivates of step (a)3O4Magnetic
Property nano-particle is nuclear core, SiO2For protection shell, shell contains the nano-particle of terminal amino group structure, super
After sound dispersion, at 25 ± 5 DEG C, react 8.5h, reaction terminate after with Magnet separation product, and use 0.1mol/L
HCl solution, second alcohol and water replace cleaning product for several times, are vacuum dried 12h, obtain adsorbent；
(2) by one block of dry soil by heavy metal pollution, crush with rotary cultivator, top layer 0.6m's
Soil breaking is less than the soil block of 3mm to diameter, and the hydrops layer irrigated to soil horizon reaches 11cm, at 25-30 DEG C
Lower stirring 12h, makes the part leaching ability of heavy metal being fixed in soil；
(3) soil after step (2) is irrigated adds the adsorbent that step (1) prepares, at 25-30 DEG C
Lower stirring 6h, then uses electromagnetism rake device to be separated by the adsorbent being adsorbed with heavy metal, and after separating
Soil in add the bodied ferric sulfate of 60mol/L with concentration be the oxalic acid solution of 0.35mol/L, both add
Entering amount is that every 40kg soil is separately added into 3kg, 4.2kg, is simultaneously introduced 0.6kg carbosphere, mechanical agitation 25min,
Stand 11h, remove supernatant, 2-3 time the most repeatedly, finally use pure water soil 1-3 time, controlled
Soil after reason.
Embodiment 4
(1) preparation of adsorbent:
A 1mol 1,4,8,11-tetraazacyclododecane tetradecane-1,4,8,11-tetraacethyl is dissolved in pH by ()
In the biological buffer of 5.3-5.5, under nitrogen protection, add 25mol catalyst EDC HCl and 9molNHS,
Stir 2h under room temperature, obtain the activated intermediate of nitrogen heterocyclic ring carboxylic acid derivates；
B () adds Fe in the activated intermediate of the prepared nitrogen heterocyclic ring carboxylic acid derivates of step (a)3O4Magnetic
Property nano-particle is nuclear core, SiO2For protection shell, shell contains the nano-particle of terminal amino group structure, super
After sound dispersion, at 25 ± 5 DEG C, react 9h, reaction terminate after with Magnet separation product, and use 0.1mol/L HCl
Solution, second alcohol and water replace cleaning product for several times, are vacuum dried 14h, obtain adsorbent；
(2) by one block of dry soil by heavy metal pollution, crush with rotary cultivator, top layer 0.7m's
Soil breaking is less than the soil block of 3mm to diameter, and the hydrops layer irrigated to soil horizon reaches 12cm, at 25-30 DEG C
Lower stirring 14h, makes the part leaching ability of heavy metal being fixed in soil；
(3) soil after step (2) is irrigated adds the adsorbent that step (1) prepares, at 25-30 DEG C
Lower stirring 7h, then uses electromagnetism rake device to be separated by the adsorbent being adsorbed with heavy metal, and after separating
Soil in add the bodied ferric sulfate of 70mol/L with concentration be the oxalic acid solution of 0.4mol/L, both add
Entering amount is that every 40kg soil is separately added into 3.5kg, 4.4kg, is simultaneously introduced 0.7kg carbosphere, mechanical agitation
30min, stands 12h, removes supernatant, 2-3 time the most repeatedly, finally uses pure water soil 1-3 time,
Soil after being governed.
Embodiment 5
(1) preparation of adsorbent:
A 1mol 1,4,7,10,13-five-nitrogen heterocyclic pentadecane-1,4,7,10,13-pentaacetic acid is dissolved in pH by ()
For in the biological buffer of 5.3-5.5, under nitrogen protection, add 30mol catalyst EDC HCl and
11molNHS, stirs 2.5h, obtains the activated intermediate of nitrogen heterocyclic ring carboxylic acid derivates under room temperature；
B () adds Fe in the activated intermediate of the prepared nitrogen heterocyclic ring carboxylic acid derivates of step (a)3O4Magnetic
Property nano-particle is nuclear core, SiO2For protection shell, shell contains the nano-particle of terminal amino group structure, super
After sound dispersion, at 25 ± 5 DEG C, react 9.5h, reaction terminate after with Magnet separation product, and use 0.1mol/L
HCl solution, second alcohol and water replace cleaning product for several times, are vacuum dried 16h, obtain adsorbent；
(2) by one block of dry soil by heavy metal pollution, crush with rotary cultivator, top layer 0.8m's
Soil breaking is less than the soil block of 3mm to diameter, and the hydrops layer irrigated to soil horizon reaches 13cm, at 25-30 DEG C
Lower stirring 16h, makes the part leaching ability of heavy metal being fixed in soil；
(3) soil after step (2) is irrigated adds the adsorbent that step (1) prepares, at 25-30 DEG C
Lower stirring 8h, then uses electromagnetism rake device to be separated by the adsorbent being adsorbed with heavy metal, and after separating
Soil in add the bodied ferric sulfate of 80mol/L with concentration be the oxalic acid solution of 0.45mol/L, both add
Entering amount is that every 40kg soil is separately added into 4kg, 4.6kg, is simultaneously introduced 0.8kg carbosphere, mechanical agitation 35min,
Stand 13h, remove supernatant, 2-3 time the most repeatedly, finally use pure water soil 1-3 time, controlled
Soil after reason.
Embodiment 6
(1) preparation of adsorbent:
A () is by molten for 1mol 1,4,7,10,13,16-hexanitrogen heterocycle octadecane-1,4,7,10,13,16-six acetic acid
Solution, in the biological buffer that pH is 5.3-5.5, under nitrogen protection, adds 35mol catalyst EDC HCl
And 13molNHS, stir 2.8h under room temperature, obtain the activated intermediate of nitrogen heterocyclic ring carboxylic acid derivates；
B () adds Fe in the activated intermediate of the prepared nitrogen heterocyclic ring carboxylic acid derivates of step (a)3O4Magnetic
Property nano-particle is nuclear core, SiO2For protection shell, shell contains the nano-particle of terminal amino group structure, super
After sound dispersion, at 25 ± 5 DEG C, react 9.5h, reaction terminate after with Magnet separation product, and use 0.1mol/L
HCl solution, second alcohol and water replace cleaning product for several times, are vacuum dried 18h, obtain adsorbent；
(2) by one block of dry soil by heavy metal pollution, crush with rotary cultivator, top layer 0.9m's
Soil breaking is less than the soil block of 3mm to diameter, and the hydrops layer irrigated to soil horizon reaches 14cm, at 25-30 DEG C
Lower stirring 18h, makes the part leaching ability of heavy metal being fixed in soil；
(3) soil after step (2) is irrigated adds the adsorbent that step (1) prepares, at 25-30 DEG C
Lower stirring 9h, then uses electromagnetism rake device to be separated by the adsorbent being adsorbed with heavy metal, and after separating
Soil in add the bodied ferric sulfate of 90mol/L with concentration be the oxalic acid solution of 0.45mol/L, both add
Entering amount is that every 40kg soil is separately added into 4.5kg, 4.8kg, is simultaneously introduced 0.9kg carbosphere, mechanical agitation
40min, stands 14h, removes supernatant, 2-3 time the most repeatedly, finally uses pure water soil 1-3 time,
Soil after being governed.
Claims (9)
1. the lossless restorative procedure of a heavy-metal contaminated soil, it is characterised in that comprise the following steps:
(1) by one block of dry soil by heavy metal pollution, crush with rotary cultivator, top layer
The soil breaking of 0.5-1m is less than the soil block of 3mm to diameter, and the hydrops layer irrigated to soil horizon reaches
10-15cm, stirs 10-20h at 25-30 DEG C, makes the part leaching ability of heavy metal being fixed in soil；
(2) soil after step (1) is irrigated adds Fe3O4For nuclear core, SiO2Receiving for shell
Rice grain is as adsorbent, and the shell edge of this core-shell structure particles is modified with nitrogen heterocyclic ring carboxylic acid and derives
Thing, stirs 5-10h at 25-30 DEG C, then uses electromagnetism rake device will be adsorbed with the absorption of heavy metal
Agent is separated, and adds buffer in the soil after separating, and is simultaneously introduced carbosphere, and machinery stirs
Mix 20-40min, stand 10-15h, remove supernatant, 2-3 time the most repeatedly, finally wash with pure water
Wash soil 1-3 time, the soil after being governed.
The lossless restorative procedure of a kind of heavy-metal contaminated soil the most as claimed in claim 1, its feature
It is, in step (2), containing atom N on the ring skeleton of described nitrogen heterocyclic ring carboxylic acid derivates, ring
Atom N on skeleton is connected with carboxyl arm, and described carboxyl arm is positioned at outside ring.
The lossless restorative procedure of a kind of heavy-metal contaminated soil the most as claimed in claim 1, its feature
Being, in step (2), described nitrogen heterocyclic ring carboxylic acid derivates is Isosorbide-5-Nitrae, 7-7-triazacyclononane-Isosorbide-5-Nitrae, 7-
Triacetic acid, Cyclen-1,4,7,10-tetraacethyl, 1,4,8,11-tetra-azepine
The ring tetradecane-1,4,8,11-tetraacethyl, 1,4,7,10,13-five-nitrogen heterocyclic pentadecane-1,4,7,10,13-
In pentaacetic acid, 1,4,7,10,13,16-hexanitrogen heterocycle octadecane-1,4,7,10,13,16-six acetic acid one
Kind.
The lossless restorative procedure of a kind of heavy-metal contaminated soil the most as claimed in claim 1, its feature
Being, in step (2), the preparation method of described adsorbent comprises the following steps:
A nitrogen heterocyclic ring carboxylic acid derivates is dissolved in the biological buffer that pH is 5.3-5.5 by (),
Under nitrogen protection, add catalyst EDC HCl and NHS, stir 1.5-3h under room temperature, obtain azepine
The activated intermediate of macro ring carboxylic acid derivates；
B () adds ammonia in the activated intermediate of the prepared nitrogen heterocyclic ring carboxylic acid derivates of step (a)
The magnetic microsphere of base functionalization, after ultrasonic disperse, reacts 8-10h, after reaction terminates at 25 ± 5 DEG C
With Magnet separation product, and replace cleaning product for several times with 0.1mol/L HCl solution, second alcohol and water,
Vacuum drying 10-20h, obtains adsorbent.
The lossless restorative procedure of a kind of heavy-metal contaminated soil the most as claimed in claim 4, its feature
Being, in step (b), the magnetic microsphere of described amino functional is with Fe3O4Magnetic nanoparticle is
Nuclear core, SiO2For protection shell, shell contains terminal amino group structure.
The lossless restorative procedure of a kind of heavy-metal contaminated soil the most as claimed in claim 4, its feature
Being, in step (a), described nitrogen heterocyclic ring carboxylic acid derivates, the mol ratio of EDC HCl, NHS are
1:(10-40): (5-15).
The lossless restorative procedure of a kind of heavy-metal contaminated soil the most as claimed in claim 4, its feature
Being, in step (a), described biological buffer solutions is the morpholino b acid aqueous solution of 1mol/L.
The lossless restorative procedure of a kind of heavy-metal contaminated soil the most as claimed in claim 1, its feature
Be, in step (2), described buffer be concentration be that the bodied ferric sulfate of 50-100mol/L is with dense
Degree is the mixture of 1:1 for the oxalic acid solution of 0.3-0.5mol/L according to volume ratio.
The lossless restorative procedure of a kind of heavy-metal contaminated soil the most as claimed in claim 1, its feature
Being, in step (2), the buffer of described addition and the volume ratio of carbosphere are (10-15): 1.
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