CN104959369A - Method used for recycling chromium from chromium-polluted soil - Google Patents
Method used for recycling chromium from chromium-polluted soil Download PDFInfo
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- CN104959369A CN104959369A CN201510258431.2A CN201510258431A CN104959369A CN 104959369 A CN104959369 A CN 104959369A CN 201510258431 A CN201510258431 A CN 201510258431A CN 104959369 A CN104959369 A CN 104959369A
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Abstract
The invention discloses a method used for recycling chromium from chromium-polluted soil. The method comprises following steps: (1) chromium in chromium-polluted soil is converted into chromium VI via oxidation; (2) a leacheate is added into the soil containing chromium VI for leaching or/and elution so as to obtain slightly toxic soil with chromium VI residue and a leacheate containing chromium VI; (3) a reducing agent is added into the slightly toxic soil so as to realize reduction of the chromium VI residue, an extraction agent is added into the leacheate containing chromium VI, and the leacheate containing chromium VI is subjected to separation so as to obtain the recycled leacheate and an organic phase loaded with chromium VI; (4) the organic phase loaded with chromium VI is subjected to reduction with an aqueous solution containing an organic reducing agent, chromium VI is converted into chromium III via reduction, chromium III is transferred into a water phase via reextraction, and a chromium III aqueous solution and a regenerated organic phase are obtained via separation; and (5) the chromium III aqueous solution is subjected to solvent evaporation and crystallization, and recycling of chromium III is realized. The method can be used for high efficiency restoration of chromium-polluted soil; no secondary pollution is caused; a sulfate is taken as a desorption agent; desorption effect is excellent; and economic benefit is excellent.
Description
Technical field
The present invention relates to a kind of technique reclaiming chromium from chromium-polluted soil.
Background technology
In natural environment, the form of common chromium has trivalent chromium and Cr VI, and the trivalent chromium in chromium-polluted soil often exists with the form of indissoluble hydroxide, general low toxicity or micro-poison, and mobility is little, and is under general condition not easily spontaneously oxidized to Cr VI; And chromic toxicity is chromic 100 times, mobility is strong, migration easier than trivalent chromium causes biological chain enrichment, solubility Cr VI has strong oxidizing property, mutagenicity and carcinogenicity, interference crop root part is to other element normal absorption and transport, by the low side upwards enrichment of food chain from biosphere, make the protein denaturation in animal body, interferases system.Cr VI is to human body mainly chronic murder by poisoning, human body is entered by approach such as skin, respiratory tract and alimentary canals, mainly accumulate in vivo in lung, liver, kidney and incretory, cause nauseating, diarrhoea, the symptom such as skin ulcer, mucous membrane damage, nasal septum hemorrhage even perforation, bronchitis, the even carcinogenic threat to life of Long Term Contact severe patient.
In recent years, on market crome metal and chromic salts in the industries such as plating, casting, chemical industry, metallurgy, leather manufacture and Aero-Space as raw material of industry extensive use, its demand increases day by day, its chromium residue produced in industrial processes near soil cause severe contamination, but effective technology of repairing chromium contaminated soil and technique are not overripened.At present, the main method of chromium-polluted soil reparation has following several:
(1) chemical cleaning method: the chromium in chromium-polluted soil is by soil particle adsorption or the chromate that is dissolved in soil pore water, utilize hydraulic head to promote cleaning fluid by chromium-polluted soil, chromium to be cleared out from soil, and then the cleaning fluid containing chromium is processed.Cleaning fluid may contain certain complexing agent, or is exactly clear water.The overall efficiency of Chemical cleaning is both relevant with the effect between cleaning agent and pollutant, also with the physicochemical properties of cleaning agent itself and soil relevant to suction-operated of pollutant, chemical etc.Chemical cleaning method expense is lower, the not direct contact stain thing of operating personnel, but is only applicable to the large soil of the infiltration coefficients such as sandy loam, and the cleaning agent introduced easily causes secondary pollution.
(2) chemical reduction method: utilize iron filings, ferrous sulfate or some other appearance facile chemical reducing agent that hexavalent chrome reduction is become trivalent chromium, form the compound of indissoluble, thus reduce the animal migration of chromium in soil and bioavailability, thus alleviate the harm of pollution of chromium.When Cr VI mainly concentrates on soil particle surface, can work quickly and effectively directly to adding reducing agent in soil, but when Cr VI is present in soil particle inside, then be difficult to contact concurrent raw reduction reaction with reducing agent.Chemical reduction method belongs to in-situ remediation method, and this method is workable, and processing cost is lower, and the oxidation product that reducing agent produces likely causes secondary pollution and is difficult to process, strengthens follow-up processing cost, and its reducing process needs further optimizing research.
(3) electro reclamation method: insert yin, yang electrode in soil, applies direct current, under electric field action, and chromate anion CrO
4 2-anode is moved, and is pumped by the chromatedsolution of anode enrichment and disposes to ground, utilizes absorption method or oxidation-reduction method to remove Cr VI, Water Spreading after purification, continue to dissolve the chromate in soil, electromigration, absorption or reduction, so circulate, make soil repaired.But its energy consumption is large, easily causes soil fertility to weaken, is applicable to the pollution of small size.
(4) biological restoration: administer chromium-polluted soil by plant and microorganism.Phytoremediation technology utilizes the chromium in its absorption chromium-polluted soil, and moved to by chromium in plant, then gather in plant and chromium is taken away soil, phytoremediation is applicable to large-area treatment, and processing cost is low, but treatment cycle is very long, is applicable to shallow-layer reparation.Microorganism remediation is by two kinds of effect solidification chromium, to reduce the harm that chromium-polluted soil causes, one is the metabolic processes by microorganism self, chromium is solidificated in microorganism in health, then by peeling off to reach the object removing chromium to the screening of microorganism; Two is pass through bioreduction, hexavalent chrome reduction is become trivalent chromium, or be the form of relative nontoxic by other poisonous Forms Transformations of chromium, it is strong that microbial method relies on searching resistance to acids and bases, the microbial strains that reproducibility is strong, the investment of this method is little, operating cost is low, non-secondary pollution, but the process chromium quantity of slag is little, and efficiency is lower.
(5) solidify stabilization method: mixed with certain adhesive by chromium-polluted soil (also can be aided with certain reducing agent, for reduction of hexavalent chromium), fix chromium wherein by the adhesive such as cement, tripoli, make chromium environmental transport and transfer no longer towards periphery.This method needs to excavate soil, and cost is higher, and needs relatively large curing agent, and curing agent is dealt with improperly and may be caused secondary pollution, deficiency in economic performance.
Both advantageous and disadvantageous to the method for chromium-polluted soil reparation above, both chromic harm is eliminated in order to reach, make to be restored by chromium-polluted soil, rare chromium resource can be allowed again to recycle, a kind of new chromium-polluted soil restorative procedure need be developed, make it reach technique is simple, treatment effeciency is high, non-secondary pollution, economic benefit are higher object.
Summary of the invention
The technical problem that the present invention solves makes that chromium-polluted soil renovation technique is simple, treatment effeciency is high, non-secondary pollution, economic benefit are higher.
Technical scheme of the present invention is, provides a kind of technique reclaiming chromium from chromium-polluted soil, comprises the following steps:
(1) in chromium-polluted soil, add oxidant, the chromium in chromium-polluted soil is oxidized to Cr VI, obtain Cr VI soil;
(2) in Cr VI soil, add leacheate to carry out leaching or/and drip washing, obtain residual chromic micro-pesticide-clay mixture earth and contain Cr VI leacheate;
(3) in micro-pesticide-clay mixture earth, add reducing agent, make the hexavalent chrome reduction remained, obtain nontoxic soil; To described containing adding extractant in Cr VI leacheate, Cr VI being enriched in organic phase and being separated, being recycled leacheate and the chromic organic phase of load;
(4) with the aqueous solution containing organic reducing agent, the chromic organic phase of described load is reduced, after making hexavalent chrome reduction become trivalent chromium, entered aqueous phase by reextraction, after two-phase laminated flow, obtain the trivalent chromium aqueous solution and regeneration organic phase; Described organic reducing agent to be carbon number the be alcohol of 1 ~ 3, one or more mixing in aldehyde and carboxylic acid;
(5) solvent evaporation post crystallization is carried out to the described trivalent chromium aqueous solution, reclaim trivalent chromium.
Further, in micro-pesticide-clay mixture earth of step (3), alkaline cementing material is also added.
Further, described alkaline cementing material is one or more in lime, waterglass and cement.
Further, described leacheate is the aqueous solution containing strippant, and described strippant is soluble sulphate.
Further, described strippant is sodium sulphate.
Further, described organic reducing agent is ethanol.
Further, described extractant is trialkyl tertiary amine.
Further, described extraction is three stage countercurrent extractions; Described back extraction is taken as three stage countercurrents and strips.
Further, described extractant and the described volume ratio containing Cr VI leacheate are 1 ︰ (20 ~ 30).
Further, described recovery leacheate returns in step (2) and uses as leacheate.
Although trivalent chromium animal migration in soil is more weak, energy stable existence is in soil, and the impact of a certain amount of trivalent chromium on environment is less.If but there is a large amount of trivalent chromiums in soil, its environmental risk coefficient is still larger.In soil, system is complicated, and trivalent chromium can be oxidized to Cr VI and enter body of groundwater under certain condition, polluted-water, and with underground water generation flowing transport, even enters biological chain, be detrimental to health.Reducing total chromium content in soil content, is one of effective measures reducing pollution of chromium risk.
The present invention is by the method for chromium a large amount of in soil by oxidation-leaching, makes it separate from soil, and reclaims chromium wherein.Reduce the chromium content in soil to greatest extent, reduce the risk factor of pollution of chromium.Remaining chromium, by reduction stabilization processes, makes it stablize and is cemented in soil, reduce the risk factor of pollution of chromium to greatest extent.The technology of concrete employing is " oxidation-leaching-waste liqouor-soil stabilization process ".First the method for oxidation is adopted to make to become Cr VI containing the trivalent chromium oxidation in chromium soil, the Cr VI in soil is gone out by leaching drip washing, Cr VI is made to enter in washing water, recycling extraction is extracted the Cr VI in washing water with reduction reextraction, is concentrated and reduce, and then obtain chromium system product and recycled, remaining Cr VI, by after reduction stabilization processes, makes to be detoxified by chromium-polluted soil.
To achieve these goals, the present invention is described in detail as follows adopted portion of techniques main points:
Chromium in soil is oxidized to Cr VI: under certain pH value condition, in chromium-polluted soil, adds the oxidant of metering, trivalent chromium oxidation is become Cr VI.Oxidant includes but not limited to that trivalent chromium oxidation can be become one or both and two or more mixing in chromic oxidant by potassium permanganate, hydrogen peroxide, hypochlorite, chlorine dioxide, perchlorate and persulfate etc., two kinds and two or more mixing time, can be arbitrary proportion mixing.When carrying out oxidation reaction, regulate the acid-base value of soil by adding acid in chromium-polluted soil, and it is stable to control acid-base value maintenance.Acid used can be one or both and the two or more mixed acid that include but not limited in hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, acetic acid etc., two kinds and two or more mixing time, can be arbitrary proportion mixing.System acid-base value is adjusted to and oxidation can be made fully to be reacted, and general adjustment hierarchy of control acid-base value (pH value) are between 4 ~ 7.
Leach or/and drip washing to the chromium-polluted soil after oxidation: in order to improve chromic extraction rate, add leacheate, leacheate comprises eluent and strippant, and eluent generally selects water; Strippant uses soluble sulphate, preferably sulfuric acid sodium.Find through overtesting, sulfate is far better relative to the desorption effect of carbonate, and can not react in acid condition, in addition its price also relative moderate.Chromium-polluted soil is leached or/and become residual a small amount of chromic micro-pesticide-clay mixture earth after drip washing.
Cr VI is exist with chromate anionic form in soil, and the commutative absorption of colloid positively charged in soil is with CrO
4 2-, HCrO
4 -, Cr
2o
7 2-the chromium anion that form exists, oxide or the hydrous oxide colloid of such as iron, aluminium have very strong suction-operated to Cr VI.These cation micelles same are to other anion as carbonate, sulfate radical, phosphate radical, arsenate etc. also have very strong suction-operated, and these anion oxyacid roots and chromate just define competitive Adsorption.That is displacement can be gone by the chromate adsorbed with these anion oxyacid roots, chromate is desorbed from positively charged micelle.Have report to think that carbonate is the strippant of very effective chromic acid chromium, we study discovery, and sulfate radical is more obvious to the desorption effect of chromate.
In addition, from the existence form of trivalent chromium soil, free state and carbonate have higher activity in conjunction with state, easily run off.So be often carry out under mildly acidic conditions when being oxidized chromic, by carbonate decomposition, the chromium making carbonate change into free state in conjunction with the chromium of state is oxidized.So use carbonate desorb to there is significant limitation.When cooking strippant with sulfate, sulfate can enter containing in chromium leacheate with leacheate, after extract and separate Cr VI, sulfate can be stayed in raffinate, drip washing is carried out to containing chromium soil with raffinate, sulfate can be made to recycle, because extraction is carried out, in acid condition so carbonate cannot use.From cost analysis, the price of sulfate is well below carbonate.Comprehensive analysis, our present sulfate is as strippant.
Extraction and reduction reextraction: take organic amine as extractant, the Cr VI collected in leacheate is extracted in organic phase, after separation, reclaim leacheate can reuse, continue on for the chromium in washed off soil, wherein, the ratio of extractant and leacheate adjusts to 1 ︰ (20 ~ 30), and in the process of extraction, Cr VI is concentrated enrichment.Then, by adding organic reducing agent, Cr VI is reduced into trivalent chromium and is stripped, and trivalent chromium is stripped in aqueous phase simultaneously, and extractant is reproduced, and recycles; Be stripped into chromium in aqueous phase and reach chemical products containing chromium through pervaporation, concentrated, crystallization, chromium is recovered utilization.
Micro-pesticide-clay mixture earth removing toxic substances: residual a small amount of chromic micro-pesticide-clay mixture earth is reduced into trivalent chromium by reducing agent, reducing agent can be inorganic reducing agent or organic reducing agent as one or both in ferrous sulfate, sulphite or oxalic acid, hydrazine hydrate, ethanol and two or more, can be arbitrary proportion during two or more mixing.Or/and after reduction, use alkaline cementing material while reduction, as adjustment acid-base values such as lime, waterglass, cement, and carry out consolidation.
The invention has the beneficial effects as follows, repair chromium-polluted soil efficiently, non-secondary pollution, use sulfate as strippant, desorption effect is better, and economic benefit is higher.
Accompanying drawing explanation
Fig. 1 represents a kind of technique reclaiming chromium from chromium-polluted soil provided by the invention.
Detailed description of the invention
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with drawings and Examples, but content of the present invention is not only confined to the following examples.Extractant N235 in embodiment is three octyl tertiary amines.
Embodiment: the present embodiment provides a kind of technique reclaiming chromium from chromium-polluted soil, as shown in Figure 1, concrete steps are as follows in technological process:
(1) the present embodiment for total chrome content in certain chromium salt factory chromium-polluted soil at 25000 ~ 30000mg/kg.PH value=10.0 ~ 10.5.Piled up after fragmentation, screening by chromium-polluted soil, compound concentration is 2%wt liquor potassic permanganate, and is 4 ~ 5 by sulfuric acid adjusted to ph.The oxidizing agent solution prepared is sprayed downwards from the soil top of piling up, collect flow out from mound bottom containing Cr VI efflux.When the amount of aqueous solution used containing oxidant reaches 5 times of soil volume, stop spray, obtain Cr VI soil.
(2) spray obtaining Cr VI soil as leacheate with the aqueous solution of contains sodium sulfate, in efflux, initial content of 6-valence Cr ions is 6000 ~ 7000mg/L, content of 6-valence Cr ions afterwards in efflux declines gradually, when content of 6-valence Cr ions in efflux is not higher than 50mg/L, stop drip washing, obtain micro-pesticide-clay mixture earth.
(3) with the mixed solution of the sodium sulfite of 2.5%wt, 1% hydrazine hydrate and 1% waterglass, drip washing is carried out to mound.Convection current water outlet detects in real time, to flow out the total chromium of water and Cr VI up to standard, stop drip washing, obtain nontoxic soil.The chromium-containing solution merging obtained containing Cr VI efflux and step (2) that step (1) is obtained, three stage countercurrent extractions are carried out with 30%N235-kerosene, namely the aqueous phase of extraction reclaims the drip washing that leacheate continues on for step (2), the oil phase of extraction and the chromic organic phase of load.Reclaim contains sodium sulfate in leacheate, partially or completely can replace leacheate.
(4) the chromic organic phase of load adds 5% ethanol water, carries out three stage countercurrent reduction reextractions, obtains regeneration organic phase and the trivalent chromium aqueous solution, and regeneration organic phase is used for the extraction in step (3).
(5) trivalent chromium be reduced enters aqueous phase, obtains the trivalent chromium aqueous solution, and the trivalent chromium aqueous solution obtains chromium sulfate product through solvent evaporation, condensing crystallizing.
Every kilogram, containing recyclable six hydrated sulfuric acid chromium 90g in chromium soil, is worth 1.15 yuan, processes one kilogram of processing cost containing chromium soil and is about 1.0 yuan.This shows, adopt technical finesse provided by the present invention containing chromium soil, the value of the chromium reclaimed is higher than processing cost (time Chromium in Soil comparision contents is high).Not only reclaim resource, but also considerably reduce integrated treatment cost.
Each raw material cited by the present invention, and the bound of each raw material of the present invention, interval value, and the bound of technological parameter (as temperature, time etc.), interval value can realize the present invention, do not enumerate embodiment at this.
Claims (10)
1. from chromium-polluted soil, reclaim a technique for chromium, it is characterized in that, comprise the following steps:
(1) in chromium-polluted soil, add oxidant, the chromium in chromium-polluted soil is oxidized to Cr VI, obtain Cr VI soil;
(2) in Cr VI soil, add leacheate to carry out leaching or/and drip washing, obtain residual chromic micro-pesticide-clay mixture earth and contain Cr VI leacheate;
(3) in micro-pesticide-clay mixture earth, add reducing agent, make the hexavalent chrome reduction remained, obtain nontoxic soil; To described containing adding extractant in Cr VI leacheate, Cr VI being enriched in organic phase and being separated, being recycled leacheate and the chromic organic phase of load;
(4) with the aqueous solution containing organic reducing agent, the chromic organic phase of described load is reduced, after making hexavalent chrome reduction become trivalent chromium, entered aqueous phase by reextraction, after two-phase laminated flow, obtain the trivalent chromium aqueous solution and regeneration organic phase; Described organic reducing agent to be carbon number the be alcohol of 1 ~ 3, one or more mixing in aldehyde and carboxylic acid;
(5) solvent evaporation post crystallization is carried out to the described trivalent chromium aqueous solution, reclaim trivalent chromium.
2. technique as claimed in claim 1, is characterized in that, in micro-pesticide-clay mixture earth of step (3), also add alkaline cementing material.
3. technique as claimed in claim 2, it is characterized in that, described alkaline cementing material is one or more in lime, waterglass and cement.
4. technique as claimed in claim 1 or 2, is characterized in that, described leacheate is the aqueous solution containing strippant, and described strippant is soluble sulphate.
5. technique as claimed in claim 4, it is characterized in that, described strippant is sodium sulphate.
6. technique as claimed in claim 1 or 2, it is characterized in that, described organic reducing agent is ethanol.
7. technique as claimed in claim 1 or 2, it is characterized in that, described extractant is trialkyl tertiary amine.
8. technique as claimed in claim 1 or 2, is characterized in that, described extraction is three stage countercurrent extractions; Described back extraction is taken as three stage countercurrents and strips.
9. technique as claimed in claim 1 or 2, is characterized in that, described extractant and the described volume ratio containing Cr VI leacheate are 1 ︰ (20 ~ 30).
10. technique as claimed in claim 1 or 2, it is characterized in that, described recovery leacheate returns in step (2) and uses as leacheate.
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| CN113828630A (en) * | 2021-10-19 | 2021-12-24 | 重庆大学 | Restoration method of hexavalent chromium contaminated soil |
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| CN113828630B (en) * | 2021-10-19 | 2022-09-09 | 重庆大学 | Restoration method of hexavalent chromium contaminated soil |
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