CN107597787A - A kind of method of waste slag containing mercury efficient stable - Google Patents
A kind of method of waste slag containing mercury efficient stable Download PDFInfo
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- CN107597787A CN107597787A CN201710686973.9A CN201710686973A CN107597787A CN 107597787 A CN107597787 A CN 107597787A CN 201710686973 A CN201710686973 A CN 201710686973A CN 107597787 A CN107597787 A CN 107597787A
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Abstract
The invention discloses a kind of method of waste slag containing mercury efficient stable, this method comprises the following steps:1) waste slag containing mercury is crushed, sieving processing, takes the lower mercury slag particulate of sieve;2) add water moisturizing in mercury slag particulate, add oxidizing agent solution, stir and heat carry out oxidation reaction;3) vulcanization salting liquid is added in mercury slag particulate and carries out vulcanization reaction;4) ferrous salt is added in mercury slag particulate and precipitates excessive S2‑, 5) and addition clay mineral and humus are adsorbed in mercury slag particulate, and 6) pH adjusting agent regulation mercury contaminated soil pH to 6~7 is added in mercury slag particulate, conserve more than 3 days;This method can carry out Simultaneous Stabilization solidification to variform mercury in waste slag containing mercury, and stabilization effect is good and the cycle is short, and the medicament stock source that this method uses is wide, cost is low, is advantageous to extensive use.
Description
Technical field
The present invention relates to a kind of heavy metal waste slag processing method, more particularly to a kind of stabilization processes for waste slag containing mercury
Method, belong to heavy metal waste slag Treatment process field.
Background technology
In recent years, developing rapidly with industrial or agricultural, mercury are largely discharged in the production and use process,《National Hazard
Waste register》Mercurous waste is classified as HW29 class hazardous wastes.Waste slag containing mercury is primarily referred to as mercury ore exploitation smelting, chlor-alkali work
The mercurous solid waste caused by industry such as industry, battery and the thermometer manufacturing.These mercurous waste mercury contents are high, if improper
Conduct oneself well and put, it will pollution air, Soil Surrounding, surface water and underground water, the mercury and mercuric compounds in soil can pass through food chain
Into human body, greatly harm is produced to human body.Therefore, suitable method is selected to carry out the safe disposal of waste slag containing mercury, to me
State's environmental improvement, protection health are significant.
The treatment technology of existing waste slag containing mercury mainly includes resource reclaim and security landfill, a kind of method of resource reclaim
It is mercury is transferred in gas phase by heat treatment, then reclaims mercury by cooling down, another method is to make mercury by chemical extraction
The methods of being transferred in liquid phase, then passing through ion exchange reclaims mercury.Resource reclaim method is because the value of the mercury of recovery is not high and locates
Reason cost is higher and is rarely applied to large-scale waste slag containing mercury and administers, the most most mature and reliables of waste slag containing mercury Treatment process application
Or security landfill, waste slag containing mercury because mercury content is higher, mostly need to by curing/stabilizing method processing after can fill out safely
Bury.Curing/stabilizing method is come the technical combinations of pollutant in immobilized waste by physics and chemical action.Stabilize and solidify
Reagent can with waste residue heavy metal contaminants occur chemically or physically react, be allowed to be converted into not readily dissolve, transfer ability is weak,
The smaller form of toxicity.The stabilization agent for mercury contaminated soil and the technique study of reparation are more in the prior art, as in
State's patent (CN105414166A) discloses a kind of restorative procedure of mercury contaminated soil, specifically by mercury contaminated soil from earth's surface
Layer soil plough turns over, and air-dries, grinds, sieves, obtains pretreated topsoil;Will be by bentonite, hydroxyapatite, thio sulphur
The passivator of sour ammonium and calcium hydroxide composition, fully mixes with treated topsoil, places 10-20 days until topsoil
The 70% of middle mercury content is fixed, and passivator reparation is completed;Topsoil is flattened and plants upper India cabbage mustard, in India mustard
Orchid growth animated period is soluble in water and be uniformly sprayed onto it in India's cabbage mustard root system surrounding soil by calcium thiosulfate, finally receives
Cut India cabbage mustard.Chinese patent (A of CN 105598145) discloses a kind of in-situ remediation method of mercury contaminated soil, this method
From three kinds of charcoal, calcium polysulfide and sodium selenite passivator, it can be effective after being applied to using charcoal mixing in soil
Improve Soil Micro-environment, in meta-alkali and the stronger soil of reproducibility, the migration of mercury substantially reduces, and has powerful ratio surface
With loose structure, complicated organo-functional group a large amount of sticking soil of charcoal and can in mercury;Vulcanize is poured in soil more
Calcium solution can further promote the mineralising of mercury, and its root soil microenvironment bioactivity is strengthened after Planting Crops, and selection applies
Sodium selenite solution, its biological effectiveness is weakened using the antagonistic effect of selenium and mercury.After adding three kinds of passivation processing, show
Work reduces mercury content in crops.Chinese patent (A of CN 104998894) discloses a kind of mercury contaminated soil solidification and stabilization
Method, including villaumite addition process, pH adjustment process, mixed processes, addition activator process, digestion molding procedure and broken place
Science and engineering sequence.This method can carry out solidification and stabilization to the mercury contaminated soil of different pollution levels, and solidification can also be cooperateed with stable
Change other heavy metals in contaminated soil.Product after solidification and stabilization can backfill or for other purposes.But for containing
Mercury waste residue belongs to mercury enrichment slag, its mercury complicated component included, and content is high, is generally adapted to repair the medicament of mercury contaminated soil
Not necessarily it is adapted to the stabilisation of waste slag containing mercury with method.
The content of the invention
The defects of for existing in the prior art to waste slag containing mercury administering method, the purpose of the present invention are intended to provide one kind
Simultaneous Stabilization solidification, and the method that stabilization effect is good and the cycle is short, the party can be carried out to variform mercury in waste slag containing mercury
Method use medicament stock source is wide, cost is low, be advantageous to extensive use.
In order to realize above-mentioned technical purpose, the invention provides a kind of method of waste slag containing mercury efficient stable, this method
Comprise the following steps:
1) waste slag containing mercury is crushed, sieving processing, takes the lower mercury slag particulate of sieve;
2) add water moisturizing in mercury slag particulate, add oxidizing agent solution, stir and heat carry out oxidation reaction;
3) sodium sulfide solution is added in mercury slag particulate and carries out vulcanization reaction;
4) ferrous salt is added in mercury slag particulate and precipitates excessive S2-;
5) add clay mineral in mercury slag particulate and humus is adsorbed;
6) pH adjusting agent regulation mercury contaminated soil pH to 6~7 is added in mercury slag particulate, is conserved more than 3 days;
Wherein,
Oxidant is measured with more than 2 times of mercury mole in waste slag containing mercury;
Sulphurizing salt is measured with more than 2 times of mercury mole in waste slag containing mercury;
Ferrous salt is with 0.5%~3% metering of waste slag containing mercury quality;
Clay mineral and humus are with 2%~15% metering of waste slag containing mercury quality;
PH adjusting agent is measured with adjusting the pH of waste slag containing mercury 6~7.
Preferable scheme, the oxidant are persulfate;More preferably it is potassium peroxydisulfate and/or sodium peroxydisulfate;Further
Preferably potassium peroxydisulfate.
Preferable scheme, the sulphurizing salt include at least one of vulcanized sodium, ammonium sulfide, potassium sulfide;It is more preferably vulcanization
Sodium.
Preferable scheme, the ferrous salt include at least one of ferrous sulfate, frerrous chloride, ferrous nitrate;More preferably
For ferrous nitrate.
Preferable scheme, the clay pit species include bentonite, zeolite, sepiolite, illite, montmorillonite, concave convex rod
At least one of.More preferably it is illite and/or montmorillonite.
Preferable scheme, the pH adjusting agent include at least one of calcium oxide, calcium hydroxide, calcium carbonate.
Preferable scheme, sieve lower mercury contaminated soil particulate particle diameter≤2cm.
Preferable scheme, curing time 3~7 days.
Preferable scheme, the temperature of oxidation reaction is 50~100 DEG C.
The general appropriate amount of acid that adds is as catalyst in the oxidizing agent solution of the present invention, and to improve oxidation efficiency, this is ability
The category that field technique personnel are appreciated that.Such as 4% or so potassium persulfate solution is added in 5% HCl solution, volume ratio
For 1:10.To guarantee the low price mercury such as the organic mercury in waste slag containing mercury and monovalence mercury being completely converted into Hg2+, in persulfate
Active ingredient is excessive with respect to mercury element in waste residue.
The sulphurizing salt of the present invention is as the reagent for stablizing mercury, in order to ensure the Hg in reaction system2+It is heavy to generate completely
Form sediment, the addition of sulphurizing salt is at least 2 with respect to the mole ratio of mercury element in waste residue:1.
The ferrous salt of the present invention mainly has three effects, and first, can be by excessive S present in reaction system2-Form precipitation,
It is molten to prevent mercuric sulphide from returning, second, excessive oxidant is consumed, by unnecessary Fe2+Oxidation generation ferric hydrous oxide colloid, then
Utilize its absorption and the further removal of mercury of co-precipitation, the 3rd, excessive Fe2+Presence waste residue environment is in reducing condition
Under, so it is more conducive to the generation of mercuric sulphide.
The clay mineral and humus of the present invention has the function that synergistic sorption Trace Mercury.
The pH adjusting agent of the present invention is controlled waste residue pH 6~7, is advantageous under conditions of being 6~7 in pH whole
System and mercuric sulphide are stabilized.
Safe place of the method for the stabilisation waste slag containing mercury that technical scheme provides primarily directed to waste slag containing mercury
Put and propose, a variety of valence state mercury are included in waste slag containing mercury, such as generally zeroth order, monovalence, the mercury of divalence can all exist simultaneously,
And the mercury of these valence states has higher toxicity.The present invention is contained using oxidant, compound stabilizer and pH adjusting agent Combined Treatment
Mercury waste residue, the mercury mainly acted synergistically on by chemical oxidation, precipitation, suction-operated etc. in waste residue, make mercury with mercuric sulphide
Stable form realize stabilize, substantially reduce migration and bioavailability of the mercury in waste residue, the stabilization of mercury turns to one
Individual chemical curing process, independent of microbial activity, so as to heavy metal toxicity, waste residue property is insensitive, and applicability is wide.
Synergistic function in the method for the present invention in oxidant, compound stabilizer and pH adjusting agent between each component is bright
It is aobvious, substantially increase the stabilization effect of mercury.Based on consideration Hg2+Easily and S2-Stable HgS is formed, first using over cure
The low price such as organic mercury in soil and monovalence mercury mercury oxidation is bivalent mercury by the oxidants such as hydrochlorate, recycles sulfide and Hg2+Reaction,
The stable mercuric sulphide precipitation of generation, but excessive S is generally needed to be added in actual process2-, to ensure that mercury is all fixed
Change, but if sulphur can excessively cause HgS further to generate a kind of soluble HgS2-, dissolve again.It is and ferrous by adding
Salt can make excessive S2-Formation FeS precipitations, while Fe2+Excessive oxidant can also be consumed, oxidation generation ferric hydrous oxide,
Ferric hydrous oxide can pass through adsorption and the co-precipitation removal of mercury;In addition, Fe2+Presence make waste residue environment be in reduction
Under the conditions of, so it is more conducive to the generation of mercuric sulphide, and highly stable permanent be present in waste residue.But excessive Fe2+It can trigger
The problem of new, hydrolysis easily occurs and discharges H+Ion, make waste residue souring:4Fe2++O2+6H2O→4FeOOH+8H+, pass through addition
Alkaline matter adjusts waste residue pH, makes waste residue pH finally stable between 6~7, this is the pH that mercury stablizing effect is best in waste residue.Separately
Outside, clay pit species and humus add can synergistic sorption residual mercury, further consolidate stabilization effect.
The medicament used during the waste slag containing mercury efficient stable of the present invention need to be according to mercury content in waste residue according to appropriate
Ratio and order add.
The medicament that the method for the present invention uses, such as sulphurizing salt, ferrous salt, clay pit species and humus material, it is
Solid granular is powdered, first adds sulphurizing salt during use, stirs and add ferrous salt after reacting a period of time, most
The sorbing materials such as clay pit species, humus are added afterwards, make sure to keep in mind after can not mixing to add together, otherwise sulphurizing salt meeting and ferrous salt
React and reduce active ingredient and cause stablizing effect to decline.
The pH adjusting agent of the present invention is the alkaline matters such as calcium oxide, calcium hydroxide, calcium carbonate, is solid powdery.
The method of the waste slag containing mercury stabilization processes of the present invention includes step in detail below:
(1) waste slag containing mercury crushed, be sized to particle diameter≤2cm, remove the debris such as larger stone;
(2) suitable quantity of water is added in waste slag containing mercury makes waste residue keep moistening, so that all kinds of reactions are preferably carried out, adds
The oxidizing agent solution (add in the form of a solution, and add appropriate amount of acid as catalyst) configured, stirs, heats 20min
(temperature control is between 50~100 degrees Celsius), organic mercury and monovalence mercury in waste residue is set to be converted into bivalent mercury;
(3) add sulphurizing salt, sulphurizing salt can add in solid form, can also wiring solution-forming add, stir,
Make the Hg in waste residue2+It is fully converted to HgS precipitations;
(4) ferrous salt (solid) is added, stirs, makes excessive S2-Form FeS precipitations, while unnecessary Fe2+Oxidation
Ferric hydrous oxide is generated, then by ferriferous oxide adsorption and the further removal of mercury of co-precipitation, and Fe2+Presence make
Whole environment be under reducing condition, so the more conducively generation of mercuric sulphide, and highly stable is present in for a long time in waste residue;
(5) clay pit species and humus are added, stirs, further consolidates stabilization effect;
(6) add alkaline matter to stir, the pH of waste residue is adjusted to 6~7, if the pH of waste residue is after above-mentioned steps
Through in 6~7 scopes, then this step can be exempted from, finally conserve 3~7 days.
Compared with the prior art, the advantageous effects that technical scheme is brought:
1) method of the invention can realize the efficient stableization processing of various form mercury in waste slag containing mercury;As Elemental Mercury,
Organic mercury, monovalence mercury etc. can be fixed effectively.
2) synergy ability of the various medicaments that method of the invention uses in use between each component is strong, right
Mercury stabilization effect in waste slag containing mercury is good.By aoxidizing, precipitating, adsorbing etc. under synergy to the stabilisation fixed effect of mercury
Significantly improve, the efficient stableization solidification of mercury can be realized.
3) the medicament stock source of method of the invention use is wide, cost is low, is advantageous to promote the use of.
4) method of the invention can realize the quick, efficient of variform mercury in waste slag containing mercury by simple operations step
It is fixed, general maintenance 3 days, preferable stablizing effect can be reached, pressed《Solid waste Leaching leaching method horizontal oscillations
Method》(HJ557-2009) leached, its leaching concentration is less than 0.25mg/L, meets《Hazard waste landfill contamination control standard》
(GB18598-2001) the concentration limitation of landfill yard is allowed access into.
5) method of the invention is fixed to the mercury in waste slag containing mercury by chemical stabilization, independent of microbial activity,
So as to heavy metal toxicity, waste residue property is insensitive, and applicability is wide.
Embodiment
Specific examples below is intended to further illustrate present invention, rather than the protection of limitation the claims in the present invention
Scope.
Embodiment 1
Tongren district Guizhou Province mercury ore is taken to smelt the waste residue left, mercury content is up to 1150mg/kg in waste residue, according to《Solid gives up
Thing Leaching leaching method sulfonitric method》(HJ/T299-2007) taken slag specimen is leached, mercury in its leachate
Concentration is 3.25mg/L, is exceeded《Hazardous waste judging standard leaching characteristic identification》(GB5085.3-2007) the concentration limit of mercury in
Value 0.1mg/L, this waste slag containing mercury are hazardous waste.According to《Solid waste Leaching leaching method horizontal vibration method》
(HJ557-2009) taken slag specimen is leached, the concentration of mercury is 1.68mg/L in its leachate, is exceeded《Hazard waste landfill
Contamination control standard》(GB18598-2001) the concentration limit 0.25mg/L of landfill yard is allowed access into, need to carry out stabilizing admittedly
Change processing reaches admissions criteria.
(1) waste slag containing mercury crushed, be sized to particle diameter≤2cm, remove the debris such as larger stone;
(2) suitable quantity of water is added in waste slag containing mercury makes it keep moistening, so that all kinds of reactions are preferably carried out, adds and matches somebody with somebody
(4% potassium persulfate solution is added in 5% HCl solution the oxidant put, volume ratio 1:10) potassium peroxydisulfate, is controlled
In active ingredient and waste residue in mercury element mol ratio be not less than 2:1, stir, heating 20min (80 take the photograph by temperature control
Family name's degree), organic mercury and monovalence mercury in waste residue is converted into bivalent mercury;
(3) 5% sodium sulfide solution is added, the addition of vulcanized sodium is the mole ratio of element sulphur and mercury element in waste residue
For 2:1, stir, react 30min, make the Hg in waste residue2+It is fully converted to HgS precipitations;
(4) ferrous nitrate is added, addition is the 2% of slag quality, is stirred, and reacts 15min;
(5) illite, montmorillonite and humus are added, the mass ratio between three is 1:1:1, total addition is soil matter
The 10% of amount, stirs;
(6) add calcium hydroxide to stir, the pH of waste residue is adjusted to 6-7, if the pH of soil is after above-mentioned steps
Through in 6-7 scopes, then this step can be exempted from;
(7) conserve 3 days after according to《Solid waste Leaching leaching method horizontal vibration method》(HJ557-2009) carry out
Leach, the concentration of mercury is 0.09mg/L in its leachate, is met《Hazard waste landfill contamination control standard》(GB18598-
2001) the concentration limitation 0.25mg/L of landfill yard is allowed access into.
Embodiment 2
Waste residue same as Example 1 is taken, and is handled through identical crushing and screening, suitable quantity of water is added in waste residue makes waste residue
Moistening is kept, adding the oxidant that has configured, (4% sodium peroxydisulfate solution is added in 5% HCl solution, and volume ratio is
1:10) mol ratio of mercury element in active ingredient and waste residue in sodium peroxydisulfate, is controlled to be not less than 2:1, stir, heat
20min (temperature control is at 80 degrees Celsius), remaining step is same as Example 1, maintenance 3 days after according to《Solid waste leaches
Toxicity leaching method horizontal vibration method》(HJ557-2009) leached, the concentration of mercury is 0.13mg/L in its leachate, is higher than
Value in embodiment 1, but can meet《Hazard waste landfill contamination control standard》(GB18598-2001) landfill is allowed access into
The concentration limitation 0.25mg/L of field.
Embodiment 3
Waste residue same as Example 1 is taken, and is handled through identical crushing and screening, adds oxidation same as Example 1
Agent carries out the same oxidation reaction, adds 5% potassium sulfide solution, the addition of potassium sulfide is element sulphur and mercury element in waste residue
Mole ratio be 2:1, stir, react 30min, add frerrous chloride, addition is the 2% of slag quality, and stirring is equal
It is even, react 15min;Add bentonite, zeolite and humus, the mass ratio between three is 1:1:1, total addition is waste residue matter
The 10% of amount, stirs;Next adjust pH the step of it is same as Example 1, maintenance 3 days after according to《Solid waste leaches poison
Property leaching method horizontal vibration method》(HJ557-2009) leached, the concentration of mercury is 0.15mg/L in its leachate, higher than reality
The value in example 1 is applied, but can be met《Hazard waste landfill contamination control standard》(GB18598-2001) landfill yard is allowed access into
Concentration limitation 0.25mg/L.
Comparative example 1
Take with the identical waste residue of case study on implementation 1, and through identical crushing and screening handle, add with the identical of case study on implementation 1
Oxidant carries out the same oxidation reaction, then adds 5% sodium sulfide solution, the addition of vulcanized sodium is element sulphur and waste residue
The mole ratio of middle mercury element is 1:1, stir, react 30min, following step is identical with case study on implementation 1, maintenance 3
After it according to《Solid waste Leaching leaching method horizontal vibration method》(HJ557-2009) leached, mercury in its leachate
Concentration be 0.38mg/L, higher than the value in case study on implementation 1, and can not meet《Hazard waste landfill contamination control standard》
(GB18598-2001) the concentration limitation of landfill yard is allowed access into.
Comparative example 2
Take with the identical waste residue of case study on implementation 1, and through identical crushing and screening handle, oxidizer is not carried out at oxidation
Reason, remaining step is identical with case study on implementation 1, maintenance 3 days after according to《Solid waste Leaching leaching method horizontal oscillations
Method》(HJ557-2009) leached, the concentration of mercury is 0.45mg/L in its leachate, higher than the value in case study on implementation 1, and not
It can meet《Hazard waste landfill contamination control standard》(GB18598-2001) the concentration limitation of landfill yard is allowed access into.
Comparative example 3
Take with the identical waste residue of case study on implementation 1, and through identical crushing and screening handle, add with the identical of case study on implementation 1
Oxidant carries out the same oxidation reaction, then adds sodium sulfide solution, ferrous nitrate, illite, montmorillonite and humic simultaneously
Matter, addition is identical with case study on implementation 1, be stirring evenly and then adding into calcium hydroxide regulation pH to 6-7, maintenance 3 days after according to《Solid
Waste Leaching leaching method horizontal vibration method》(HJ557-2009) leached, the concentration of mercury is in its leachate
0.82mg/L, far above the value in case study on implementation 1, and it can not meet《Hazard waste landfill contamination control standard》(GB18598-
2001) the concentration limitation of landfill yard is allowed access into.
Claims (10)
- A kind of 1. method of waste slag containing mercury efficient stable, it is characterised in that:Comprise the following steps:1) waste slag containing mercury is crushed, sieving processing, takes the lower mercury slag particulate of sieve;2) add water moisturizing in mercury slag particulate, add oxidizing agent solution, stir and heat carry out oxidation reaction;3) vulcanization salting liquid is added in mercury slag particulate and carries out vulcanization reaction;4) ferrous salt is added in mercury slag particulate and precipitates excessive S2-;5) add clay mineral in mercury slag particulate and humus is adsorbed;6) pH adjusting agent regulation mercury contaminated soil pH to 6~7 is added in mercury slag particulate, is conserved more than 3 days;Wherein,Oxidant is measured with more than 2 times of mercury mole in waste slag containing mercury;Sulphurizing salt is measured with more than 2 times of mercury mole in waste slag containing mercury;Ferrous salt is with 0.5%~3% metering of waste slag containing mercury quality;Clay mineral and humus are with 2%~15% metering of waste slag containing mercury quality;PH adjusting agent is measured with adjusting the pH of waste slag containing mercury 6~7.
- 2. the method for waste slag containing mercury efficient stable according to claim 1, it is characterised in that:The oxidant is over cure Hydrochlorate.
- 3. the method for waste slag containing mercury efficient stable according to claim 2, it is characterised in that:The oxidant included Potassium sulfate and/or sodium peroxydisulfate.
- 4. the method for waste slag containing mercury efficient stable according to claim 1, it is characterised in that:The sulphurizing salt includes sulphur Change at least one of sodium, ammonium sulfide, potassium sulfide.
- 5. the method for waste slag containing mercury efficient stable according to claim 1, it is characterised in that:The ferrous salt includes sulphur At least one of sour ferrous iron, frerrous chloride, ferrous nitrate.
- 6. the method for waste slag containing mercury efficient stable according to claim 1, it is characterised in that:The clay pit species bag Include at least one of bentonite, zeolite, sepiolite, illite, montmorillonite, concave convex rod.
- 7. the method for waste slag containing mercury efficient stable according to claim 1, it is characterised in that:The pH adjusting agent includes At least one of calcium oxide, calcium hydroxide, calcium carbonate.
- 8. the method for the waste slag containing mercury efficient stable according to any one of claim 1~7, it is characterised in that:The lower mercury of sieve Slag particulate particle diameter≤2cm.
- 9. the method for the waste slag containing mercury efficient stable according to any one of claim 1~7, it is characterised in that:During maintenance Between be 3~7 days.
- 10. the method for the waste slag containing mercury efficient stable according to any one of claim 1~7, it is characterised in that:Oxidation is anti- The temperature answered is 50~100 DEG C.
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CN108405599A (en) * | 2018-03-27 | 2018-08-17 | 中交天航环保工程有限公司 | One heavy metal species and cyanide polluted composite soil repairing method |
CN111570469A (en) * | 2020-05-13 | 2020-08-25 | 中信环境技术(广州)有限公司 | Treatment method of mercury-containing waste |
CN112961679A (en) * | 2021-02-01 | 2021-06-15 | 博天环境集团股份有限公司 | Repairing agent and method for stably repairing mercury-polluted soil by adopting same |
CN114713594A (en) * | 2022-04-07 | 2022-07-08 | 生态环境部南京环境科学研究所 | Molten slag utilization device for hazardous waste incineration and use method thereof |
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