CN104927870B - soil repairing agent and preparation method and use method thereof - Google Patents
soil repairing agent and preparation method and use method thereof Download PDFInfo
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- CN104927870B CN104927870B CN201510301965.9A CN201510301965A CN104927870B CN 104927870 B CN104927870 B CN 104927870B CN 201510301965 A CN201510301965 A CN 201510301965A CN 104927870 B CN104927870 B CN 104927870B
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Abstract
The invention discloses a soil remediation agent and a preparation method and a use method thereof. The material comprises: 5-15% of modified carbon nano tube, 10-60% of modified clay mineral and 20-60% of quicklime. The S-CrPbCd can efficiently adsorb Pb, Cd and Cr in soil without remarkably changing soil property and tiltability. The residual quantity of Pb, Cd and Cr in sensitive crops can be reduced by 75-90% within 1-2 months by S-CrPbCd, and meanwhile, the material has the characteristics of low cost, simple preparation process, no secondary pollution, quick response, easy large-area popularization and the like.
Description
Technical field
The invention belongs to field of environmental improvement, it is related to the improvement of heavy metal pollution, specifically a kind of soil-repairing agent
And preparation method thereof and using method.
Background technology
For many years, the discharge of three industrial wastes, domestic waste, mud and containing the pesticide of heavy metal, chemical fertilizer unreasonable
Use, make soil contaminated, wherein, heavy metal pollution has become as one of environmental problem of sternness.Grind in environmental pollution
In studying carefully, heavy metal, referring to the significant chemical element of the bio-toxicity such as Hg, Cd, Pb, Cr and metalloid As more.Heavy metal pollution of soil
Yield and the quality of crops can be affected, and the health of the mankind can be endangered by food chain.
Simple substance chromium（Cr）It is a kind of stable metal, be widely used in rustless steel processed, auto parts, instrument, tape and video recording
Band etc., chromium is plated on metal can be antirust, firm attractive in appearance.Cr is trace element needed by human, and it controls metabolism with other
Material coordinates and has an effect, such as hormone, insulin, various enzyme, the genetic stew of cell（DNA and RNA）Deng.Cr is synthesis
The necessary raw material of some human hormones, Cr3+It is to human body beneficial element, and Cr6+It is Z toxic element.In wholefood,
The content of Cr is typically relatively low and be all with Cr3+Form exists.The impact to absorption of human body for the form of Cr is very big, and human body is to inorganic
Chrome uptake ability is extremely weak, and utilization rate is less than 1%；And the utilization rate to organic chromium is 10-25%.Therefore, often using rich Cr medium-height grass
Cr deficiency disease treated by medicine, can obtain satisfied effect, excessive Cr is to human body toxic side effect, but the toxicity of Cr is had with its valence state
Close.Cr6+Toxicity be about Cr3+100 times of toxicity.The Cr of excess intake, can lead to Cr long-term accumulation in vivo.According to
Relative national standards, Cr in varieties of food items3+Content be usually no more than 1.0ppm, but can arrive in aquatic animal and milk powder
2.0ppm.
Heavy metal Pb and Cd are the environmental contaminants with the features such as high poison, non-degradable and biological concentration.Heavy metal Pb master
The nervous system of human body to be encroached on；The hormonal system such as Cd main harm human skeleton system and kidney.
At present, heavy metal pollution of soil restorative procedure mainly include elution method, stabilizing method, heavy metal pollution of soil, electrokinetic process and
Phytoremediation etc..According to Environmental Protection Agency USA（USEPA）Recommendation, stabilizing method be soil heavy metal combined pollution administer
A most effective, most economical class method.Clay mineral is often used as the raw material of renovation agent, for example：Zeolite is a kind of aqueous
The rack-like aluminium silicate mineral of alkali and alkaline earth metal ions, has a lot of cavitys and duct so as to have very strong in crystal structure
Adsorption；Zeolite crystal skeleton cationic and skeleton contact weaker, easily generation cation exchange.Montmorillonite is by two-layer
Silicon-oxy tetrahedron presss from both sides 2 that one layer of alumina octahedral is constituted:1 type phyllosilicate, has larger surface area and pore volume, in structure cell
In structure, isomorphous substitution can occur so as to have stronger ion exchangeable and water absorption.However, natural zeolite and montmorillonite
Because there is Free water, absorption water, constitution water and water of crystallization, and the presence of the symbiosis impurity of significant proportion in mineral, weaken
Overall physical and chemical performance, so that its colloidality, adsorptivity etc. are greatly affected in actual applications.
Patent CN 104031651 A discloses a kind of heavy metal pollution farmland that is used for and is passivated modifying agent and its using method.
Its raw material includes flyash, nanometer iron powder, zeolite, Maifanitum, calcium magnesium phosphate, hydroxypropyl modified SiO2/ chitosan nano particle
With hole nodular fibrous element.This composite passivated modifying agent can improve the passivation effect to the heavy metal chromium in soil, cadmium, lead, arsenic
Really.This passivation modifying agent can improve to heavy metal in soil cadmium, lead, chromium passivation effect, make soil available Cd, lead,
Chromium reduces by 43.3% ~ 67.2%, 44.5% ~ 59.4% and 31.6% ~ 71.7% respectively；The Chinese cabbage of plantation in soil after process, inhales
The cadmium of receipts, lead, chromium content reduce 52.9% ~ 63.9%, 46.3% ~ 63.6% and 34.9% ~ 60.9% respectively.
Patent CN 104004524 A discloses the environment-friendly type administered with a kind of soil remediation for industrial pollution place
Heavy metal stabilizer and its using method.This stabilizer preparation method, according to mass fraction meter, comprises following material composition：Clay
40 ~ 50 parts of mineral, 10 ~ 18 parts of heavy metal chelant, 4 ~ 8 parts of heavy metal precipitator, 10 ~ 15 parts of alkaline conditioner.This stabilizer
Can be used for the heavy metals such as chromium in fixing soil, cadmium, lead, copper, nickel.After in soil after process, total cadmium content is reduced to≤manages
In soil total cadmium be reduced to containing total lead content≤lead content is reduced to total cadmium, total lead content is reduced to≤15 mg/L, substantially reduces
Its toxicity, meets the regulation of leaching characteristic identification standard value（GB5085.6-2007）Regulation, reach place the set goal and repair
Complex value（The 10% of toxicity judging standard value）Repairing effect and requirement.
Patent CN 101962553 A discloses a kind of firming agent for the reparation by heavy-metal contaminated soil, each group
Point percentage by weight be：Cement 25% ~ 40%, high adsorption clay mineral 40% ~ 65%, quick lime 10% ~ 20%.This firming agent pair
Heavy metal lead, zinc, cadmium have good fixed effect.Using high adsorption clay mineral replacing partial cement, flyash and calculogenesis
Ash etc. to soil fail obvious firming agent although the heavy metal ion such as cadmium, lead can be fixed, but still suffer from destroy the soil body knot
Structure, cause secondary pollution equivalent risk.
Patent CN 104046361 A discloses with a kind of compound heavy metal contaminated soil conditioner and its application and applies
Use method.The weight proportion that it comprises component is：Plant ash：Calcium magnesium phosphate：Quick lime：Zeolite：Hydroxyapatite：Fertilizer=
（0.3-1.1）：（0.1-0.2）：（0.4-2.1）：（0.1-0.6）：（0.008-0.06）：（0.4-1.2）.In actual applications,
This compound heavy metal contaminated soil conditioner coordinates microbial function bacterium solution, can improve Soil structure, be passivated and repair dirt
Various heavy in dye soil, such as chromium, lead, cadmium, manganese etc..
Patent CN 103894402 A discloses a kind of method of soil decontamination containing Cr VI, and the method is passed through to by sexavalence
Repeatedly add the reducing agents such as sulphite in the soil of pollution of chromium, and the firming agent such as sulphurizing salt and lime water, effectively degraded and
Have cured the chromium in soil.
Mostly there is following defect in the existing repair materials for heavy-metal contaminated soil process：（1）Repair materials are originally
Body just be enough to the various heavy polluting containing concentration, easily causes secondary pollution；（2）The materials such as renovation agent raw material such as cement
Material then can cause soil compaction, the plantation function of impact soil；（3）Renovation agent needs to use the gold belonging to organic pollution in itself
Belong to chelating agen, after chelating agen degraded, heavy metal discharges again；（4）The raw material types of renovation agent are various, preparation technology
Complexity, high cost.
Therefore, research and development repairing effect is obvious, with low cost, technological process is simple, repairing efficiency is short, applied widely, no
Destroying Soil structure and plantation function, the new material of non-secondary pollution is this area technical barrier urgently to be resolved hurrily.
Content of the invention
The technical problem to be solved in the present invention is：A kind of new material S- of remediating heavy metal Cr-Pb-Cd contaminated soil is provided
CrPbCd and its using method, to improve to the heavy metal lead in soil, cadmium, the repairing effect of chromium.CNT and clay pit
Thing has excellent physicochemical characteristic, is prepared by modification, and its heavy metal Cr, Pb and Cd are provided simultaneously with powerful stabilisation effect
Really.
Raw material of the present invention does not contain harmful heavy metal or other harmful substances, and its raw material includes modified carbon nano tube
Pipe, modified zeolite and modified montmorillonite used mixture, quick lime.The renovation agent that the present invention provides is combined solid preparation, is named as
" S-CrPbCd ", for the meaning of " chromium, lead and cadmium stabilizer ".
CNT preferably has the activated carbon of nano tubular structure, its adsorbable different types of heavy metal, carbon nanometer
Pipe increased its hydrophilic and the ion-exchange capacity to heavy metal in soil through superoxidized modified process, has greatly than table
Area and abundant pore structure.
Zeolite after peracid, heat modification and montmorillonite, not only solvable go in carbonate impurity and crystal structure duct
Other cationes of absorption, remove the impurity being distributed in duct, so that duct is dredged, increase pore volume；Clay mineral also can be made
Lose the combination water in surface water, water of hydration and structural framework, reduce the absorbability of moisture film heavy metal pollutant, strengthen viscous
The absorption property of native mineral.
Quick lime, provides more stable slight alkali environment, in the basic conditions, easy and Pb2+、Cd2+、Cr6+Form indissoluble multiple
Compound, thus reduce the biological effectiveness of Pb, Cd, Cr and transportable property；On the other hand, quick lime can make on the pH value of soil
Rise 0.2 about but do not significantly change soil property and farming it is also possible to prevent the loss of soil nutrient.
The technical scheme that the present invention is adopted by its technical problem of solution is as follows：
A kind of new material S-CrPbCd of remediating heavy metal Cr-Pb-Cd contaminated soil is it is characterised in that each component is pressed such as
Lower percentage by weight composition：Modified carbon nano-tube 5% ~ 15%, modified clay mineral 10% ~ 60% and quick lime 20% ~ 60%.
Wherein, the method for modifying of described modified carbon nano-tube includes：
The first step, the potassium permanganate of CNT, 65% concentrated nitric acid, 0.5 mol/L is pressed mass fraction for 1：2：5
Ratio mixes, stands and cools down；
Second step, the material after above-mentioned cooling is aoxidized 2 h at 90 DEG C, and centrifugal filtration simultaneously cools down；
3rd step, deionized water cyclic washing is centrifuged, until supernatant pH stable；
4th step, dries at 60 ~ 80 DEG C to constant weight amount, grinds, obtain modified carbon nano-tube.
Wherein, described modified clay mineral is modified zeolite and modified montmorillonite used compositionss, described modified zeolite and modification
The method of modifying of montmorillonite includes：
The first step, pretreatment：Natural zeolite and montmorillonite are spontaneously dried, is ground into powder respectively with mortar, and mistake
200 mesh sieve screenings, obtain zeolite and montmorillonite pretreatment product；
Second step, acid is modified：Weigh zeolite after pretreatment and montmorillonite, being separately added into concentration is 3 mol/L HNO3
Solution, solid-to-liquid ratio is 1:3, temperature control at 70 ~ 80 DEG C, soaking and stirring 2 h, and be aided with ultrasonic Treatment；Centrifugal filtration, cooling
Afterwards, it is washed with deionized to neutrality, activation 2 hs are dried under the conditions of 105 DEG C；
3rd step, heat modification：Zeolite after will be acid-modified and montmorillonite carry out heat treatment, and heat modification temperature is respectively：
250 ~ 500 DEG C of zeolite, 300 ~ 650 DEG C of montmorillonite, after heat modification 2 ~ 4 h, are respectively put into cooling in exsiccator；
4th step, mixing：By the zeolite after peracid, heat modification and montmorillonite according to（2~5）：（1~3）Weight proportion
Mixing, stirs.
The invention provides the preparation method of new material, including：
The first step, as described above the method for modifying of modified carbon nano-tube prepare modified carbon nano-tube；
Second step, modified zeolite and modified montmorillonite used method of modifying prepare modified zeolite and modified illiteracy as described above
De- stone；
3rd step, by each component according to modified carbon nano-tube 5% ~ 15%, modified clay mineral 10% ~ 60% and quick lime 20% ~
60% weight ratio is uniformly mixed, that is, obtain described new material S-CrPbCd.
A kind of using method of the new material S-CrPbCd of remediating heavy metal Cr-Pb-Cd contaminated soil, described using method
Using following operating procedure：
The first step, pretreatment：For nonirrigated farmland, 0 ~ 20 cm arable layer contaminated soil is dug out, remove the large volume in soil
The debris such as branch, gravel, and large volume aggravation of soil is carried out broken it is desirable to diameter of soil pellet is less than 1 cm；For paddy field,
Can typically be turned over operation；
Second step, renovation agent dispensing：S-CrPbCd, S- are added according to the soil weight, cultivated area and arable layer thickness
CrPbCd adding proportion is the 0.1% ~ 1.0% of contaminated soil weight；
3rd step, mixing：For nonirrigated farmland, heavy-metal composite pollution soil is sufficiently stirred for by available blender with S-CrPbCd
After uniformly, then plus 10% ~ 20% pollution-free clean water is sufficiently stirred for；For paddy field, the soil surface after turning over covers above-mentioned
S-CrPbCd and soil are fully mixed by appropriate S-CrPbCd again by the mode turned over, stir；
4th step, soil reaction：Soil backfill original place after processing, keeps 10% ~ 20% moisture content to place 1 month,
S-CrPbCd is made fully to react with heavy metal, after sample detecting is qualified, you can normal plantation.
Wherein, described second step S-CrPbCd adding proportion is the 0.3% ~ 0.5% of contaminated soil weight.
Wherein, the ratio of each component of described S-CrPbCd changes with the change of Heavy Metals in Soil Contaminated concentration, but its model
Enclose less than modified carbon nano-tube 5% ~ 15%, modified clay mineral 10% ~ 60% and quick lime 20% ~ 60%.
Wherein, to compound heavy metal chromium, lead, add described new material S-CrPbCd in the soil of cadmium pollution.
Beneficial effect using technical scheme is：
First, new material S-CrPbCd repairing effect substantially and has higher stability, after applying S-CrPbCd, sensitive
In plant, Pb, Cd, Cr residual quantity can reduce by 75% ~ 90%；.
Second, S-CrPbCd raw material sources are extensively, with low cost, and 1/3rd of about external congenic method；
3rd, renovation technique flow process is simple, can combine with general farming activity；
4th, S-CrPbCd are applied widely, can be applicable to Pb, Cd, Cr pollution mine soil reparation and farming land reparation
In field it is easy to spread；
5th, repairing efficiency is short, does not destroy Soil structure and plantation function, non-secondary pollution, repairing effect are lasting.
Brief description
Fig. 1 is the preparation technology flow chart of heavy metal-polluted soil repair materials S-CrPbCd of the present invention.
Fig. 2 is the use flow chart of the present invention.
Specific embodiment
The specific embodiment of the present invention is described below in conjunction with the accompanying drawings.
Embodiment 1
The preparation of first step modified carbon nano-tube
The potassium permanganate taking CNT, 65% concentrated nitric acid and 0.5 mol/L is 1 by mass fraction：2：5 ratio is mixed
Close uniform, standing cooling, the material after cooling is aoxidized after 2 h under the conditions of 90 DEG C, centrifugal filtration simultaneously cools down, deionized water
Cyclic washing is centrifuged, until supernatant pH is in neutrality, dries to constant weight amount, grinds, cross 200 mesh sieves, obtain carbon modified at 80 DEG C
Nanotube, modified carbon nano-tube is placed in exsiccator and preserves.
Second step modified natural zeolite and the preparation of montmorillonite
Natural zeolite and montmorillonite are spontaneously dried, is ground into powder respectively with mortar, and cross 200 mesh sieve screenings, obtain
To zeolite and montmorillonite pretreatment product, concentration is added to be 3 mol/L respectively in zeolite after pretreatment and montmorillonite
HNO3Solution, solid-to-liquid ratio is 1:3, temperature control at 80 DEG C, soaking and stirring 2 h, and be aided with supersound process, centrifugal filtration, cooling
Afterwards, be washed with deionized to neutrality, under the conditions of 105 DEG C be dried activation 2 h, will be acid-modified after zeolite and montmorillonite enter
Row heat treatment, heat modification temperature is respectively 300 DEG C of zeolite, 450 DEG C of montmorillonite, is respectively put in exsiccator cooling after 2 h, will be through
Zeolite after peracid, heat modification and montmorillonite are according to 3:2 weight proportion mixing, stirs.
The preparation of the 3rd step S-CrPbCd
Modified carbon nano-tube 10%, modified clay mineral 30% and quick lime 60% are weighed by above-mentioned mass percent, is stirring
Mix continuously stirred 1 h in device, fully mix, obtain combining renovation agent S-CrPbCd.
4th step S-CrPbCd is used for repairing Beijing Cr, Cd, Pb combined contamination soil
New material S-CrPbCd is used for repairing Beijing industrial pollution plot.Soil pH value is about 6.5, heavy metal Cr
Average content is 627 mg/kg, Cd average contents is 342 mg/kg for 1.52 mg/kg, Pb average contents.Research area belongs to
The bad three class soil of Cr, Cd and Pb Compound Heavy Metals.Renovation technique flow process such as Fig. 2, specific application process is as follows：
（1）Pretreatment：Using excavator, contaminated soil is dug out, 0 ~ 20 cm arable layer contaminated soil is dug out, remove soil
The debris such as the large volume branch in earth, gravel, and large volume aggravation of soil is crushed, diameter of soil pellet is less than 1 cm；
（2）Renovation agent dispensing：According to the soil weight, cultivated area and arable layer thickness, in contaminated soil, add quality
Fraction is 0.3% S-CrPbCd；
（3）Mixing：After contaminated soil and S-CrPbCd being stirred with blender, then plus 20% pollution-free clean
Water purification is sufficiently stirred for；
（4）Soil reaction：Will process after soil backfill original place, keep 20% about moisture content place 1 month so that
S-CrPbCd is fully reacted with Pb, Cd, Cr.
Grown on soil Herba Spinaciae after repairing through S-CrPbCd, Brassica oleracea L.var.capitata and 3 kinds of crops of Chinese cabbage, concrete operation method
As follows：
（1）Full from granularity from the seed bought, seed of uniform size is sowed；
（2）In the growth course of crop, the work such as daily watering, thinning, fertilizer and applications of pesticide is produced with local
Custom is consistent with Agriculture production and management of a family measure；The weather of daily time recording experimental situation, temperature（Daytime, night）, humidity etc.；
（3）Taken at regular intervals plant sample, carries out the analysis of the index of quality such as the residual quantity of heavy metal Cd, Cr and Pb.
After testing, in Mobile Forms heavy metal, Herba Spinaciae and Chinese cabbage in soil, Cd, Cr and Pb content all has significantly than matched group
Degree declines, and Heavy Metals In Vegetables residual quantity is minimum to decline about 75.6%, and highest declines about 91.5%, is shown in Table 1.
After reparation, in Herba Spinaciae and Chinese cabbage, the content of heavy metal is less than People's Republic of China's national food safety standard
《GB 2762-2012 pollutants in food is limited the quantity》The limitation of defined.
Table 1 S-CrPbCd is used for repairing the effect of Beijing Cd, Pb, Cr combined contamination soil
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any those familiar with the art the invention discloses technical scope in, the change or replacement that can readily occur in,
All should be included within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Enclose and be defined.
Claims (7)
1. a kind of soil-repairing agent, each component forms as following weight percent：Modified carbon nano-tube 5% ~ 15%, modified clay pit
Thing 10% ~ 60% and quick lime 20% ~ 60% it is characterised in that：Described CNT is selected from the activated carbon with nano tubular structure,
The method of modifying of described modified carbon nano-tube includes：
The first step, the potassium permanganate that CNT, 65% concentrated nitric acid, concentration are 0.5 mol/L is 1 by mass fraction：2：5
Ratio mix, standing and cool down；
Second step, the mixture after above-mentioned cooling is aoxidized after 2 h under the conditions of 90 DEG C, and centrifugal filtration simultaneously cools down；
3rd step, deionized water cyclic washing is centrifuged, until supernatant pH stable；
4th step, dries at 60 ~ 80 DEG C to constant weight, grinds, obtain modified carbon nano-tube；
Described modified clay mineral is the modified zeolite and modified montmorillonite used mixture after peracid modification and heat modification.
2. a kind of soil-repairing agent according to right 1 it is characterised in that：Described modified zeolite and modified montmorillonite used modification
Method includes：
The first step, pretreatment：Natural zeolite and montmorillonite are spontaneously dried, is ground into powder respectively with mortar, and cross 200 mesh
Sieve screening, obtains zeolite and montmorillonite pretreatment product；
Second step, acid is modified：Weigh zeolite after pretreatment and montmorillonite, being separately added into concentration is 3 mol/L HNO3Solution,
Solid-to-liquid ratio is 1:3, temperature control at 70 ~ 80 DEG C, soaking and stirring 2 h, and be aided with supersound process, after centrifugal filtration, cooling, spend
Ion water washing, to neutral, is dried activation 2 h under the conditions of 105 DEG C；
3rd step, heat modification：Zeolite after will be acid-modified and montmorillonite carry out heat treatment, and heat modification temperature is respectively zeolite
250 ~ 500 DEG C, 300 ~ 650 DEG C of montmorillonite, after heat modification 2 ~ 4 h, are respectively put into cooling in exsiccator；
4th step, mixing：By the zeolite after peracid, heat modification and montmorillonite according to（2~5）：（1~3）Weight proportion mixing,
Stir, obtain modified zeolite and modified montmorillonite used mixture.
3. a kind of soil-repairing agent according to right 1 or 2 is it is characterised in that to compound heavy metal chromium, lead, cadmium pollution
Soil in add described soil-repairing agent.
4. a kind of preparation method of soil-repairing agent is it is characterised in that include：
The first step, prepares modified carbon nano-tube in accordance with the method for claim 1；
Second step, prepares modified zeolite and modified montmorillonite used in accordance with the method for claim 2；
3rd step, each component is uniformly mixed according to the weight ratio described in claim 1, that is, obtains described soil remediation
Agent.
5. a kind of using method of soil-repairing agent is it is characterised in that include：
The first step, pretreatment：For nonirrigated farmland, 0 ~ 20cm arable layer contaminated soil is dug out, remove soil in large volume branch,
The debris such as gravel, carry out broken so that diameter of soil pellet is less than 1 cm to large volume aggravation of soil；For paddy field, one can be carried out
As turn over operation；
Second step, renovation agent dispensing：Soil-repairing agent is added according to the soil weight, cultivated area and arable layer thickness, soil is repaiied
Multiple agent adding proportion is the 0.1% ~ 1.0% of contaminated soil weight；
3rd step, mixing：For nonirrigated farmland, heavy-metal composite pollution soil and soil-repairing agent are sufficiently stirred for all by available blender
After even, then plus 10% ~ 20% pollution-free clean water is sufficiently stirred for；For paddy field, the soil surface after turning over covers adaptability of soil earth
Soil-repairing agent and soil are fully mixed by renovation agent again by the mode turned over, stir；
4th step, soil reaction：Soil backfill original place after processing, keeps 10% ~ 20% moisture content to place 1 month, makes soil
Earth renovation agent and heavy metal are fully reacted, and can normally plant after sample detecting is qualified.
6. according to claim 5 the using method of soil-repairing agent it is characterised in that described second step soil-repairing agent adds
Plus ratio is the 0.3% ~ 0.5% of contaminated soil weight.
7. according to right 5 or 6 using method of soil-repairing agent it is characterised in that described soil-repairing agent each component
Ratio changes with the change of Heavy Metals in Soil Contaminated concentration, but its scope is less than claim 1.
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