CN104927870A - Novel material for repairing heavy metal Cr-Pb-Cd polluted soil, and preparation method and application method thereof - Google Patents
Novel material for repairing heavy metal Cr-Pb-Cd polluted soil, and preparation method and application method thereof Download PDFInfo
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Abstract
The invention discloses a new material S-CrPbCd for repairing heavy metal Cr-Pb-Cd polluted soil, 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, relate to the improvement of heavy metal contamination, specifically a kind of novel material and preparation method thereof of remediating heavy metal Cr-Pb-Cd contaminated soil and using method.
Background technology
For many years, the discharge of three industrial wastes, domestic waste, mud and containing the agricultural chemicals of heavy metal, the unreasonable use of chemical fertilizer, make soil receive pollution, and wherein, heavy metal contamination has become one of severe environmental problem.In Study on environmental pollution, the significant chemical elements of bio-toxicity such as heavy metal many fingers Hg, Cd, Pb, Cr and metalloid As.Heavy metal pollution of soil can affect the seed output and quality of farm crop, and by the health of food chain harm humans.
Simple substance chromium (Cr) is a kind of stable metal, and be widely used in stainless steel processed, auto parts, instrument, tape and video-tape etc., chromium is plated in can be antirust on metal, firm attractive in appearance.Cr is the trace element of needed by human, and it coordinates with other material controlling metabolism and has an effect, as the genetic stew (DNA and RNA) etc. of hormone, Regular Insulin, various enzyme, cell.Cr is the necessary raw material of some human hormone of synthesis, Cr
3+to human body beneficial element, and Cr
6+it is Z toxic element.In whole food, the content of Cr is general lower and be all with Cr
3+form exists.The form of Cr is very large on the impact of absorption of human body, and human body is extremely weak to the receptivity of inorganic chromium, and utilization ratio is less than 1%; And be 10-25% to the utilization ratio of organic chromium.Therefore, often utilize rich Cr Chinese herbal treatment Cr deficiency disease, can obtain satisfied effect, excessive Cr is to human body toxic side effect, but the toxicity of Cr is relevant with its valence state.Cr
6+toxicity be approximately Cr
3+100 times of toxicity.The Cr of excess intake, can cause Cr long-term accumulation in vivo.According to relative national standards, Cr in varieties of food items
3+content be generally no more than 1.0ppm, but can 2.0ppm be arrived in aquatic animal and milk powder.
Heavy metal Pb and Cd have high poison, do not degrade and the environmental pollutant of the feature such as biomagnification.Heavy metal Pb mainly encroaches on the neural system of human body; The endocrine systems such as Cd main harm human skeleton system and kidney.
At present, heavy metal pollution of soil restorative procedure mainly comprises drip-rinsing process, stabilizing method, soil moved in improve the original method, electrokinetic process and phytoremediation etc.According to the recommendation of USEPA (USEPA), stabilizing method is effective, the most most economical class methods that soil heavy metal combined pollution is administered.Clay mineral is often used as the starting material of renovation agent, such as: zeolite is a kind of rack-like aluminium silicate mineral of moisture alkali and alkaline earth metal ions, has a lot of cavitys and duct in crystalline structure, makes it have very strong adsorption; Zeolite crystal skeleton cationic and skeleton contact more weak, easily cationic exchange occur.Montmorillonite presss from both sides by two-layer silicon-oxy tetrahedron the 2:1 type layered silicate that one deck alumina octahedral forms, and has larger surface-area and pore volume, in cell configuration, isomorphous substitution can occur, make it have stronger ion exchangeable and water-absorbent.But, because there is free water, planar water, water of constitution and crystal water in natural zeolite and montmorillonite mineral, and the existence of the symbiosis impurity of significant proportion, weaken overall physical and chemical performance, thus its colloidality, adsorptivity etc. are greatly affected in actual applications.
Patent CN 104031651 A discloses a kind of for heavy metal contamination farmland passivation modifying agent and using method thereof.Its raw material comprises flyash, nanometer iron powder, zeolite, medical stone, fused(calcium magnesium)phosphate, hydroxypropyl modified SiO2/ chitosan nano particle and hole nodular fibrous element.This composite passivated modifying agent can improve the passivation effect to the heavy metal chromium in soil, cadmium, lead, arsenic.This passivation modifying agent can improve the passivation effect to heavy metal in soil cadmium, lead, chromium, makes soil available Cd, lead, chromium reduce by 43.3% ~ 67.2%, 44.5% ~ 59.4% and 31.6% ~ 71.7% respectively; The Chinese cabbage planted in soil after process, the cadmium of absorption, lead, chromium content reduce 52.9% ~ 63.9%, 46.3% ~ 63.6% and 34.9% ~ 60.9% respectively.
Patent CN 104004524 A discloses with a kind of environment-friendly type heavy metal stabilizer of the improvement of the soil remediation for industrial pollution place and using method thereof.This stablizer preparation method, according to mass fraction meter, comprises following material composition: clay mineral 40 ~ 50 parts, heavy metal chelant 10 ~ 18 parts, heavy metal precipitator 4 ~ 8 parts, alkaline conditioner 10 ~ 15 parts.This stablizer can be used for the heavy metal such as chromium, cadmium, lead, copper, nickel in fixing soil.In soil after process total cadmium content be reduced to≤manage after soil in total cadmium containing total lead content be reduced to≤lead content is reduced to total cadmium, total lead content is reduced to≤15 mg/L, greatly reduce its toxicity, meet the regulation of the regulation (GB5085.6-2007) of leaching characteristic identification standard value, reach repairing effect and the requirement of place the set goal reparation value (10% of toxicity judging standard value).
Patent CN 101962553 A discloses a kind of solidifying agent of the reparation for being subject to heavy-metal contaminated soil, and the weight percent of each component is: cement 25% ~ 40%, high absorbability clay mineral 40% ~ 65%, unslaked lime 10% ~ 20%.This solidifying agent heavy metal lead, zinc, cadmium have good fixed effect.Adopt high absorbability clay mineral replacing partial cement, flyash and unslaked lime etc. to the obvious solidifying agent of soil fail, although can fix the heavy metal ion such as cadmium, lead, but still existence destroys soil structures, causes secondary pollution equivalent risk.
Patent CN 104046361 A discloses with the compound heavy metal contaminated soil conditioner of one and application thereof and application process.Its weight proportion comprising component is: plant ash: fused(calcium magnesium)phosphate: unslaked 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 liquid, can improve Soil structure, passivation various heavy in repairing polluted soil, as chromium, lead, cadmium, manganese etc.
Patent CN 103894402 A discloses a kind of containing sexavalent chrome method of soil decontamination, the method is passed through to being subject to repeatedly adding the reductive agents such as sulphite in hexavalent chromium polluted soil, and the solidifying agent such as sulphide salt and liming, effectively degrade and have cured the chromium in soil.
There is following defect in the existing repair materials for heavy-metal contaminated soil process: (1) repair materials is inherently enough to the various heavy polluted containing concentration, easily cause secondary pollution mostly; (2) renovation agent starting material such as the materials such as cement then can cause soil compaction, affect the plantation function of soil; (3) renovation agent needs to use the metal chelator itself belonging to organic pollutant, and after sequestrant degraded, heavy metal discharges again; (4) various, the complicated process of preparation of the raw material types of renovation agent, cost is high.
Therefore, research and develop that repairing effect is obvious, with low cost, technical process is simple, repairing efficiency is short, applied widely, not spoiled soil structure and plantation function, non-secondary pollution novel material is this area technical barrier urgently to be resolved hurrily.
Summary of the invention
The technical problem to be solved in the present invention is: the novel material S-CrPbCd and the using method thereof that provide a kind of remediating heavy metal Cr-Pb-Cd contaminated soil, to improve the heavy metal lead in soil, and cadmium, the repairing effect of chromium.Carbon nanotube and clay mineral have excellent physicochemical characteristic, are prepared by modification, and its heavy metal Cr, Pb and Cd possess powerful stabilization effect simultaneously.
Starting material of the present invention are not containing harmful heavy metal or other objectionable impuritiess, and its raw material comprises modified carbon nano-tube, modified zeolite and modified montmorillonite used mixture, unslaked lime.Renovation agent provided by the invention is combined solid preparation, called after " S-CrPbCd ", is the meaning of " chromium, lead and cadmium stabilizer ".
Carbon nanotube preferably has the gac of nano tubular structure, its adsorbable different types of heavy metal, carbon nanotube adds its wetting ability and the ion-exchange capacity to heavy metal in soil through superoxidized modified process, has great specific surface area and abundant pore structure.
Zeolite after peracid, heat modification and montmorillonite, other positively charged ion not only adsorbed in solvable carbon elimination Barbiturates impurity and crystalline structure duct, removes the impurity be distributed in duct, duct is dredged, enlarged hole volume; Clay mineral also can be made to lose Bound moisture in surface water, water of hydration and structural framework, reduce the adsorptive power of moisture film heavy metal pollutent, strengthen the absorption property of clay mineral.
Unslaked lime, provides more stable slight alkali environment, in the basic conditions, and easy and Pb
2+, Cd
2+, Cr
6+form insoluble complex, thus reduce the biological effectiveness of Pb, Cd, Cr and transportable property; On the other hand, unslaked lime can make the pH value rising about 0.2 of soil but significantly not change soil property and farming, also can prevent the loss of soil nutrient.
The technical scheme that the present invention adopts for its technical problem of solution is as follows:
A novel material S-CrPbCd for remediating heavy metal Cr-Pb-Cd contaminated soil, is characterized in that, each component forms as following weight percent: modified carbon nano-tube 5% ~ 15%, modified clay mineral 10% ~ 60% and unslaked lime 20% ~ 60%.
Wherein, the method for modifying of described modified carbon nano-tube comprises:
The first step, the ratio being 1:2:5 in mass fraction by carbon nanotube, the concentrated nitric acid of 65%, the potassium permanganate of 0.5 mol/L mixes, leaves standstill and cooling;
Second step, is oxidized 2 h by above-mentioned cooled material at 90 DEG C, and centrifuging also cools;
3rd step, centrifugal with deionized water repetitive scrubbing, until supernatant liquor pH value is stablized;
4th step, dries to constant weight amount at 60 ~ 80 DEG C, and grinding, obtains modified carbon nano-tube.
Wherein, described modified clay mineral is modified zeolite and modified montmorillonite used composition, and described modified zeolite and modified montmorillonite used method of modifying comprise:
The first step, pre-treatment: by natural zeolite and montmorillonite seasoning, be ground into powder respectively with mortar, and cross 200 mesh sieve screenings, obtain zeolite and montmorillonite pretreatment product;
Second step, sour modification: take zeolite after pretreatment and montmorillonite, adding concentration is respectively 3 mol/L HNO
3solution (pH=4.0), solid-to-liquid ratio is 1:3, and temperature controls at 70 ~ 80 DEG C, soaking and stirring 2 h, and is aided with ultrasonication; After centrifuging, cooling, with deionized water wash to neutral, dry activation 2 h under 105 DEG C of conditions;
3rd step, heat modification: heat-treat through the modified zeolite of acid and montmorillonite, heat modification temperature is respectively: 250 ~ 500 DEG C, zeolite, montmorillonite 300 ~ 650 DEG C, after heat modification 2 ~ 4 h, puts into moisture eliminator respectively and cools;
4th step, mixing: by the zeolite after peracid, heat modification and montmorillonite according to (2 ~ 5): the weight proportion mixing of (1 ~ 3), stirs.
The invention provides the preparation method of novel material, comprising:
The first step, prepares modified carbon nano-tube according to the method for modifying of modified carbon nano-tube mentioned above;
Second step, prepares modified zeolite and modified montmorillonite used according to modified zeolite mentioned above and modified montmorillonite used method of modifying;
3rd step, is uniformly mixed the weight ratio of each component according to modified carbon nano-tube 5% ~ 15%, modified clay mineral 10% ~ 60% and unslaked lime 20% ~ 60%, namely obtains described novel material S-CrPbCd.
A using method of the novel material S-CrPbCd of remediating heavy metal Cr-Pb-Cd contaminated soil, described using method adopts following operation steps:
The first step, pre-treatment: for nonirrigated farmland, digs out 0 ~ 20 cm arable layer contaminated soil, removes the foreign material such as large volume branch, gravel in soil, and carries out fragmentation to large volume aggravation of soil, require that diameter of soil pellet is less than 1 cm; For paddy field, operation of can generally turning over;
Second step, renovation agent is prepared burden: add S-CrPbCd according to the soil weight, cultivated area and arable layer thickness, S-CrPbCd adding proportion is 0.1% ~ 1.0% of contaminated soil weight;
3rd step, mixing: for nonirrigated farmland, after heavy-metal composite pollution soil and S-CrPbCd stir by available stirrer, the more pollution-free clean water adding 10% ~ 20% fully stirs; For paddy field, the soil surface after turning over covers above-mentioned appropriate S-CrPbCd, and S-CrPbCd and soil fully mix by the mode again by turning over, stirring;
4th step, soil reaction: by the soil backfill original place after process, keep the water ratio of 10% ~ 20% to place 1 month, S-CrPbCd and heavy metal are fully reacted, after sample detecting is qualified, can normally plant.
Wherein, described second step S-CrPbCd adding proportion is 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 scope is no more than modified carbon nano-tube 5% ~ 15%, modified clay mineral 10% ~ 60% and unslaked lime 20% ~ 60%.
Wherein, to compound heavy metal chromium, plumbous, add described novel material S-CrPbCd in the soil of cadmium pollution.
The beneficial effect of technical scheme of the present invention is adopted to be:
The first, novel material S-CrPbCd repairing effect is obvious and have higher stability, and after using S-CrPbCd, in sensitive plant, Pb, Cd, Cr residual quantity can reduce by 75% ~ 90%; .
The second, S-CrPbCd raw material sources is extensive, with low cost, is about 1/3rd of external congenic method;
3rd, renovation technique flow process is simple, can combine with general farming activity;
Four, S-CrPbCd is applied widely, can be applicable to Pb, Cd, Cr and pollute the field such as mine soil reparation and farming land reparation, be easy to spread;
5th, repairing efficiency is short, and spoiled soil structure and plantation function, non-secondary pollution, repairing effect are not lasting.
Accompanying drawing explanation
Fig. 1 is preparation technology's schema of heavy metal-polluted soil repair materials S-CrPbCd of the present invention.
Fig. 2 is use schema of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described.
Embodiment 1
The preparation of the first step modified carbon nano-tube
Get carbon nanotube, the concentrated nitric acid of 65% and the potassium permanganate of 0.5 mol/L to mix in the ratio that mass fraction is 1:2:5, leave standstill cooling, after cooled material is oxidized 2 h under 90 DEG C of conditions, centrifuging also cools, centrifugal with deionized water repetitive scrubbing, until supernatant liquor pH is in neutral, dry at 80 DEG C to constant weight amount, grinding, cross 200 mesh sieves, obtain modified carbon nano-tube, modified carbon nano-tube is placed in moisture eliminator and preserves.
The preparation of second step modified natural zeolite and montmorillonite
By natural zeolite and montmorillonite seasoning, be ground into powder respectively with mortar, and cross 200 mesh sieve screenings, obtaining zeolite and montmorillonite pretreatment product, is 3 mol/L HNO respectively to adding concentration in zeolite after pretreatment and montmorillonite
3solution (pH=4.0), solid-to-liquid ratio is 1:3, temperature controls at 80 DEG C, soaking and stirring 2 h, and be aided with supersound process, after centrifuging, cooling, with deionized water wash to neutral, dry activation 2 h under 105 DEG C of conditions, heat-treat through the modified zeolite of acid and montmorillonite, heat modification temperature is respectively 300 DEG C, zeolite, montmorillonite 450 DEG C, puts into moisture eliminator respectively and cool after 2 h, zeolite after peracid, heat modification and montmorillonite are mixed according to the weight proportion of 3:2, stirs.
The preparation of the 3rd step S-CrPbCd
Modified carbon nano-tube 10%, modified clay mineral 30% and unslaked lime 60% are taken by above-mentioned mass percent, in whipping appts, Keep agitation 1 h, fully mixes, and obtains combination renovation agent S-CrPbCd.
4th step S-CrPbCd is for repairing Beijing Cr, Cd, Pb combined contamination soil
Novel material S-CrPbCd is used for repair industrial pollution plot, Beijing.Soil pH value is about 6.5, and the average content of heavy metal Cr is 627 mg/kg, Cd average contents be 1.52 mg/kg, Pb average contents is 342 mg/kg.Study area belongs to the bad three class soil of Cr, Cd and Pb Compound Heavy Metals.Renovation technique flow process is as Fig. 2, and concrete application method is as follows:
(1) pre-treatment: adopt excavator to be dug out by contaminated soil, dug out by 0 ~ 20 cm arable layer contaminated soil, remove the foreign material such as large volume branch, gravel in soil, and carry out fragmentation to large volume aggravation of soil, diameter of soil pellet is less than 1 cm;
(2) renovation agent batching: according to the soil weight, cultivated area and arable layer thickness, add the S-CrPbCd that massfraction is 0.3% in contaminated soil;
(3) mix: after contaminated soil and S-CrPbCd being stirred with stirrer, the more pollution-free clean water adding 20% fully stirs;
(4) soil reaction: by the soil backfill original place after process, keep the water ratio of about 20% to place 1 month, make S-CrPbCd and Pb, Cd, Cr fully react.
Grown on soil spinach after repairing through S-CrPbCd, Brassica oleracea L.var.capitata and Chinese cabbage 3 kinds of crops, concrete operation method is as follows:
(1) from the seed bought, select granularity full, seed of uniform size is sowed;
(2) in the process of growth of crop, the work such as daily watering, thinning, fertilizer and the applications of pesticide with local produce be accustomed to and Agriculture production and management of a family measure consistent; Every day time recording experimental situation weather, temperature (daytime, night), humidity etc.;
(3) taken at regular intervals plant sample, carries out the quality parameter analysis such as residual quantity of heavy metal Cd, Cr and Pb.
After testing, in soil, in Mobile Forms heavy metal, spinach and Chinese cabbage, Cd, Cr and Pb content all has than control group and significantly declines, and Heavy Metals In Vegetables residual quantity is minimum declines about 75.6%, and the highest decline about 91.5%, in table 1.
After reparation, in spinach and Chinese cabbage, the content of heavy metal is lower than the limitation of People's Republic of China's national food safety standard " GB 2762-2012 pollutants in food limitation " defined.
Table 1 S-CrPbCd is for repairing the effect of Beijing Cd, Pb, Cr combined contamination soil
The above; be only the present invention's preferably embodiment, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (8)
1. a novel material S-CrPbCd for remediating heavy metal Cr-Pb-Cd contaminated soil, is characterized in that, each component forms as following weight percent: modified carbon nano-tube 5% ~ 15%, modified clay mineral 10% ~ 60% and unslaked lime 20% ~ 60%.
2. the novel material S-CrPbCd of a kind of remediating heavy metal Cr-Pb-Cd contaminated soil according to claim 1, it is characterized in that, described carbon nanotube is selected from the gac with nano tubular structure, and the method for modifying of described modified carbon nano-tube comprises:
The first step, by carbon nanotube, 65% concentrated nitric acid, concentration be 0.5 mol/L potassium permanganate in mass fraction be 1:2:5 ratio mixing, leave standstill and cooling;
Second step, after above-mentioned cooled mixture is oxidized 2 h under 90 DEG C of conditions, centrifuging also cools;
3rd step, centrifugal with deionized water repetitive scrubbing, until supernatant liquor pH value is stablized;
4th step, dries to constant weight at 60 ~ 80 DEG C, and grinding, obtains modified carbon nano-tube.
3. the novel material S-CrPbCd of a kind of remediating heavy metal Cr-Pb-Cd contaminated soil according to claim 1, it is characterized in that, described modified clay mineral is modified zeolite and modified montmorillonite used mixture, and described modified zeolite and modified montmorillonite used method of modifying comprise:
The first step, pre-treatment: by natural zeolite and montmorillonite seasoning, be ground into powder respectively with mortar, and cross 200 mesh sieve screenings, obtain zeolite and montmorillonite pretreatment product;
Second step, sour modification: take zeolite after pretreatment and montmorillonite, adding concentration is respectively 3 mol/L HNO
3solution (pH=4.0), solid-to-liquid ratio is 1:3, and temperature controls at 70 ~ 80 DEG C, soaking and stirring 2 h, and is aided with supersound process, after centrifuging, cooling, with deionized water wash to neutral, dry activation 2 h under 105 DEG C of conditions;
3rd step, heat modification: heat-treat through the modified zeolite of acid and montmorillonite, heat modification temperature is respectively 250 ~ 500 DEG C, zeolite, montmorillonite 300 ~ 650 DEG C, after heat modification 2 ~ 4 h, puts into moisture eliminator respectively and cools;
4th step, mixing: by the zeolite after peracid, heat modification and montmorillonite according to (2 ~ 5): the weight proportion mixing of (1 ~ 3), stirs, obtain modified zeolite and modified montmorillonite used mixture.
4., according to the novel material S-CrPbCd of a kind of remediating heavy metal Cr-Pb-Cd contaminated soil one of right 1 to 3 Suo Shu, it is characterized in that, to compound heavy metal chromium, plumbous, add described novel material S-CrPbCd in the soil of cadmium pollution.
5. a preparation method of the novel material S-CrPbCd of remediating heavy metal Cr-Pb-Cd contaminated soil, is characterized in that, comprising:
The first step, prepares modified carbon nano-tube in accordance with the method for claim 2;
Second step, prepares modified zeolite and modified montmorillonite used in accordance with the method for claim 3;
3rd step, is uniformly mixed each component according to weight ratio according to claim 1, namely obtains described novel material S-CrPbCd.
6. a using method of the novel material S-CrPbCd of remediating heavy metal Cr-Pb-Cd contaminated soil, is characterized in that, comprising:
The first step, pre-treatment: for nonirrigated farmland, digs out 0 ~ 20cm arable layer contaminated soil, removes the foreign material such as large volume branch, gravel in soil, carries out fragmentation to make diameter of soil pellet be less than 1 cm to large volume aggravation of soil; For paddy field, operation of can generally turning over;
Second step, renovation agent is prepared burden: add S-CrPbCd according to the soil weight, cultivated area and arable layer thickness, S-CrPbCd adding proportion is 0.1% ~ 1.0% of contaminated soil weight;
3rd step, mixing: for nonirrigated farmland, after heavy-metal composite pollution soil and S-CrPbCd stir by available stirrer, the more pollution-free clean water adding 10% ~ 20% fully stirs; For paddy field, the soil surface after turning over covers appropriate S-CrPbCd, and S-CrPbCd and soil fully mix by the mode again by turning over, stirring;
4th step, soil reaction: by the soil backfill original place after process, keep the water ratio of 10% ~ 20% to place 1 month, S-CrPbCd and heavy metal are fully reacted, can normally plant after sample detecting is qualified.
7. the using method of the novel material S-CrPbCd of a kind of remediating heavy metal Cr-Pb-Cd contaminated soil according to claim 6, is characterized in that, described second step S-CrPbCd adding proportion is 0.3% ~ 0.5% of contaminated soil weight.
8. the using method of the novel material S-CrPbCd of a kind of remediating heavy metal Cr-Pb-Cd contaminated soil according to right 6 or 7, it is characterized in that, the ratio of each component of described S-CrPbCd changes with the change of Heavy Metals in Soil Contaminated concentration, but its scope is no more than claim 1.
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