CN108114972B - Method for ex-situ remediation of mercury contaminated soil - Google Patents
Method for ex-situ remediation of mercury contaminated soil Download PDFInfo
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- CN108114972B CN108114972B CN201711390792.8A CN201711390792A CN108114972B CN 108114972 B CN108114972 B CN 108114972B CN 201711390792 A CN201711390792 A CN 201711390792A CN 108114972 B CN108114972 B CN 108114972B
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- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
- B09C1/08—Reclamation of contaminated soil chemically
- B09C1/085—Reclamation of contaminated soil chemically electrochemically, e.g. by electrokinetics
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Abstract
The invention relates to a method for ex-situ remediation of mercury contaminated soil, which comprises the following steps: the method comprises the steps of excavating mercury-containing soil in layers, conveying and metering the mercury-containing soil, performing filter pressing after pre-dipping reaction to perform solid-liquid separation, enabling filter cakes generated by separation to enter a slurrying tank to perform slurrying, then entering an ore pulp electrolytic tank, homogenizing ore pulp by compressed air and stirring, introducing direct current to the cathode and the anode of the ore pulp electrolytic tank, and enabling mercurous chloride to flow out of the bottom of the ore pulp electrolytic tank due to insolubility of a solution after the ore pulp is electrolyzed to obtain a product after treatment. By utilizing the electrochemical principle, the suspension electrolysis method and the characteristic that the cathode generates the mercurous sulfide insoluble electrolyte, the mercury content of the purified soil is reduced to be below 0.1mg/kg, the extraction rate of the mercury exceeds 99.9 percent, and the adaptability is strong; the processing period is short, and the method is safe and reliable.
Description
Technical Field
The invention relates to the technical field of heavy metal contaminated soil remediation, in particular to a method for ex-situ remediation of mercury contaminated soil.
Background
The national soil pollution condition survey bulletin shows that the national soil environment condition is not optimistic overall, the soil pollution of partial areas is heavy, the quality of the cultivated land soil environment is great, and the soil environment problem of industrial and mining abandoned lands is prominent. The total overproof rate of the national soil is 16.1 percent, wherein the proportion of slightly, moderately and severely polluted points is 11.2 percent, 2.3 percent, 1.5 percent and 1.1 percent respectively. The pollution type is mainly inorganic type, the organic type is secondary, the specific gravity of the composite type pollution is small, and the number of the superstandard points of the inorganic pollutants accounts for 82.8 percent of the total superstandard points. Wherein the point standard exceeding rate of 8 inorganic pollutants of cadmium, mercury, arsenic, copper, lead, chromium, zinc and nickel is respectively 7.0%, 1.6%, 2.7%, 2.1%, 1.5%, 1.1%, 0.9% and 4.8%. The heavy metal pollution of soil has the characteristics of concealment, long-term property and irreversibility, directly or indirectly pollutes underground water and air, harms crops and organisms, and even endangers the health and the life of human beings. Therefore, repairing the heavy metal contaminated soil and recovering the original functions of the soil are always hot research tasks at home and abroad.
For heavy metal contaminated soil, there are many remediation methods at home and abroad, which are mainly classified into physical methods, physicochemical methods and the like. The main physical methods at present are the clay method, the thermal desorption method, the solidification/stabilization method, the electric restoration method and the like. The soil dressing method can be considered as a fundamental approach for thoroughly improving the soil, and has the defects of great engineering quantity and consumption, and damage to the basic structure and fertility of the original soil to a certain extent. The thermal desorption method can effectively reduce the polluted soil and avoid secondary pollution, but has the defects of high energy consumption and limited treatment capacity, and is more suitable for purifying high-concentration point pollution sources. The solidification/stabilization technology can effectively reduce the activity of heavy metals in soil, control the migration of mercury in polluted areas, has relatively moderate treatment cost, aims at soil pollutants which are mainly inorganic substances (including radioactive substances) and are generally not suitable for treating organic matters and pesticide pollution, does not fundamentally solve the pollution problem, and can release the pollutants again along with the change of the environment. The physical and chemical remediation is to add a modifier into the soil, and reduce the bioavailability and the mobility of the heavy metals through the adsorption, oxidation reduction, antagonism or precipitation of the heavy metals. A
The current chemical method is a main repair method, and the mechanism of the method is roughly as follows: regulating soil pH, chemical precipitation, organic complexation, ion exchange, etc. A method for regulating and controlling the pH value of soil: the bone meal (the main component is decacalcium phosphate), the alkali coal slag, the lime and the blast furnace have a certain adjusting effect on the pH value of the soil, but the repairing effect is not ideal. Physical and chemical fixation: the restoration agent adopted by the physical and chemical fixation method is economical, cheap and low in cost, can effectively prevent plants from absorbing mercury, but cannot fundamentally remove mercury from soil. The plant restoration method comprises the following steps: the plants purify the heavy metals in the soil through the functions of enrichment, volatilization, root filtration, stabilization and the like, and compared with the traditional physical and physical chemical technical means, the method has the advantages of convenient actual operation, small investment, no secondary pollution, easy generation of certain economic benefit and the like, but the heavy metal-enriched plants have the problems of treatment and secondary pollution.
In conclusion, various treatment technologies have certain limitations, and development of feasible heavy metal contaminated soil treatment and remediation technologies is very important.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a process method for ex-situ remediation of mercury-contaminated soil, which realizes the thorough removal of mercury from the contaminated soil, shortens the technical process, reduces the unit treatment cost, can adjust the treatment scale as required, has safe and reliable treatment process and does not generate secondary pollution.
The purpose of the invention is realized by the following technical scheme: a method for ex-situ remediation of mercury contaminated soil is characterized by comprising the following steps:
(1) after being excavated in layers, conveyed and metered, mercury-containing soil enters a pre-soaking reactor, and is subjected to pre-soaking reaction and filter pressing for solid-liquid separation, so that filter cakes and filtrate are separated;
(2) the filtrate generated by solid-liquid separation in the step (1) is subjected to mercury removal to generate a mercury sulfide product, and the mercury-removed liquid returns to the pre-soaking reactor;
(3) filter cakes generated by solid-liquid separation in the step (1) enter a slurrying tank for slurrying, then enter an ore pulp electrolytic tank, air is changed into compressed air through an air compressor and enters the ore pulp electrolytic tank, and meanwhile, ore pulp is stirred between a cathode and an anode through a stirrer to keep the ore pulp uniform;
(4) after the ore pulp electrolytic cell is prepared in the step (3), after the ore pulp is homogenized by compressed air and stirring, the ore pulp is prevented from being layered, then direct current is introduced into the cathode and the anode of the ore pulp electrolytic cell, and the ore pulp electrolysis condition is as follows: the anode is a graphite polar plate, and the cathode is a stainless steel or aluminum plate; the effective area ratio of the anode to the cathode is as follows: 1.5-2: 1; the anode current density was: 400-500A/m2And the cathode current density is: 800-1000A/m2(ii) a The catholyte comprises mixed solution of sodium chloride and hydrochloric acid, wherein the concentration of sodium chloride is 20-30g/L, and the concentration of hydrochloric acid is 10-15 g/L; the component of the anolyte is sodium chloride solution, and the concentration of the sodium chloride solution is 50-60 g/L; the anode diaphragm bag is made of polypropylene or polytetrafluoroethylene materials, the electrolysis time is three to four electrolysis cycles, and each electrolysis cycle is 3 to 6 hours; after the ore pulp is electrolyzed, the mercurous chloride discharged from the bottom of the tank flows out from the bottom of the ore pulp electrolytic tank because the mercurous chloride is insoluble in solution, and the product is obtained after treatment; the slurry flows out from the side surface of the ore pulp electrolytic tank, the slurry is subjected to solid-liquid separation through filter pressing, and the leachate enters a catholyte storage tank and then enters a replenishment head tank through conveying; the solution in the elevated tank enters the ore pulp electrolytic tank under the action of gravity;
(5) detecting and judging the purified soil, and backfilling after the purified soil is qualified; the unqualified pulp is returned to the pulping tank for further treatment.
In the technical scheme, the pre-soaking reaction liquid in the step (1) is a mixed liquid of sodium chloride and hydrochloric acid, wherein the concentration of the sodium chloride is 20-30g/L, and the concentration of the hydrochloric acid is 10-15 g/L; the solid-to-solid mass ratio of the presoaking reaction liquid is as follows: 5-7: 1; the reaction time is 120-180 min; the stirring speed is as follows: 120 to 150 rpm.
In the technical scheme, the mercury removing agent in the step (2) is sodium sulfide, and the adding amount is 3-5% of the excessive reaction amount.
In the technical scheme, the liquid-solid mass ratio of the filter cake in the step (3) entering a slurrying tank for slurrying is 8-10: 1; the compression multiple of the compressed air is 15-20 times; the stirring speed is 20-30 rpm.
In the technical scheme, the slurry in the step (4) is subjected to filter pressing twice, a filter cake obtained after the first filter pressing stays in a filter press and needs to be washed for 3-5 times, and when the pH value of filtrate is within the range of 6-8, the filter pressing is carried out again.
The invention has the beneficial effects that: the method for ex-situ remediation of mercury contaminated soil utilizes the electrochemical principle, the suspension electrolysis method and the characteristic that the cathode generates mercurous sulfide insoluble electrolyte, the mercury content of the purified soil is reduced to be below 0.1mg/kg, the extraction rate of mercury exceeds 99.9 percent, and after the reaction is finished, the average mercury content in the electrolyte is 8 multiplied by 10-2 mg/L or less; the method has short flow, low investment and low unit treatment cost; the process is clean, and no secondary pollution is generated; the processing scale can be large or small, and the adaptability is strong; the processing period is short, and the method is safe and reliable.
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In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a process flow diagram of a method for ex-situ remediation of mercury contaminated soil according to an embodiment of the invention.
Detailed Description
Example 1
The process of the ex-situ remediation method for mercury contaminated soil adopted in this embodiment is shown in fig. 1, and includes the following steps:
(1) taking 100kg of mercury-containing soil below a certain regenerated mercury enterprise, feeding the mercury-containing soil into a pre-soaking reactor, performing solid-liquid separation after pre-soaking reaction, and separating out a filter cake and filtrate; the pre-soaking reaction liquid is a mixed liquid of sodium chloride and hydrochloric acid, wherein the concentration of the sodium chloride is 25-30g/L, and the concentration of the hydrochloric acid is 10-12 g/L; the solid-to-solid mass ratio of the presoaking reaction liquid is as follows: 5-6: 1; the reaction time is 120-140 min; the stirring speed is as follows: 120 rpm;
(2) the filtrate generated by the solid-liquid separation is subjected to mercury removal to generate a mercury sulfide product, wherein the mercury removal agent is sodium sulfide, and the addition amount of the mercury removal agent is 4% of the excessive reaction amount;
(3) the filter cake generated by the solid-liquid separation enters a slurrying tank for slurrying, and the mass ratio of liquid to solid is 8: 1; meanwhile, air is changed into compressed air through an air compressor and also enters the ore pulp electrolytic cell; the compression multiple of compressed air is 16 times; meanwhile, stirring is carried out between the cathode and the anode through a stirrer, and the stirring speed is 23 rpm;
(4) and (3) introducing direct current to the cathode and the anode of the ore pulp electrolytic cell, wherein the ore pulp electrolysis conditions are as follows: the anode is a graphite polar plate, and the cathode is a graphite electrode; the effective area ratio of the anode to the cathode is as follows: 1.5: 1; the anode current density was: 400-500A/m2And the cathode current density is: 600-750A/m2(ii) a The cathode electrolyte comprises a mixed solution of sodium chloride and hydrochloric acid, wherein the concentration of the sodium chloride is 23-26g/L, and the concentration of the hydrochloric acid is 10-12 g/L; the anode electrolyte is a sodium chloride solution, and the concentration of the sodium chloride solution is 50-55 g/L; the anode diaphragm bag is made of polypropylene; three cycles of ore pulp electrolysis, wherein each electrolysis cycle is 5 hours, and mercurous chloride flows out from the bottom of the ore pulp electrolysis tank and becomes a product after treatment; the slurry flows out from the side surface of the ore pulp electrolytic cell; carrying out solid-liquid separation on the slurry through filter pressing, and conveying the leachate into a catholyte storage tank and a replenishment elevated tank; the solution in the elevated tank enters the ore pulp electrolytic tank under the action of gravity;
(5) detecting and judging the purified soil, and backfilling after the purified soil is qualified; the unqualified pulp is returned to the pulping tank for further treatment.
The results of the ex-situ remediation of mercury contaminated soil are shown in table 1.
Table 1 shows the results of the treatment of ex-situ remediation of mercury contaminated soil in example 1.
Example 2
The process of the ex-situ remediation method for mercury contaminated soil adopted in this embodiment is shown in fig. 1, and includes the following steps:
(1) taking mercury-containing soil from a chlor-alkali chemical enterprise, feeding the mercury-containing soil into a presoaking reactor, carrying out solid-liquid separation after presoaking reaction, and separating out a filter cake and filtrate; the pre-soaking reaction liquid is a mixed liquid of sodium chloride and hydrochloric acid, wherein the concentration of the sodium chloride is 26g/L, and the concentration of the hydrochloric acid is 12 g/L; the mass ratio of the presoaking reaction liquid to the solid is 6: 1; the reaction time is 125 min; the stirring speed is 140 rpm;
(2) the filtrate generated by the solid-liquid separation is subjected to mercury removal to generate a mercury sulfide product, wherein the mercury removal agent is sodium sulfide, and the addition amount of the mercury removal agent is 5% of the excessive reaction amount;
(3) the filter cake generated by the solid-liquid separation enters a slurrying tank for slurrying, and the mass ratio of liquid to solid is 9: 1; meanwhile, air is changed into compressed air through an air compressor and also enters the ore pulp electrolytic cell; the compression multiple of the compressed air is 17 times; meanwhile, stirring is carried out between the cathode and the anode through a stirrer, and the stirring speed is 25 rpm;
(4) and (3) introducing direct current to the cathode and the anode of the ore pulp electrolytic cell, wherein the ore pulp electrolysis conditions are as follows: the anode is a graphite polar plate, and the cathode is an aluminum alloy plate; the effective area ratio of the anode to the cathode is 2: 1; the anode current density was: 500A/m2And the cathode current density is 1000A/m2(ii) a The catholyte comprises mixed solution of sodium chloride and hydrochloric acid, wherein the concentration of sodium chloride is 23-26g/L, and the concentration of hydrochloric acid is 12-15 g/L; the components of the anolyte are sodium chloride solution, and the concentration of the sodium chloride solution is 55-57 g/L;the anode diaphragm bag is made of polytetrafluoroethylene. The ore pulp is electrolyzed for 4 periods, each period is 6 hours, the mercurous chloride flows out from the bottom of the ore pulp electrolytic tank, and the product is formed after treatment; the slurry flows out from the side surface of the ore pulp electrolytic cell; carrying out solid-liquid separation on the slurry through filter pressing, and conveying the leachate into a catholyte storage tank and a replenishment elevated tank; the solution in the elevated tank enters the pulp electrolytic tank through the action of gravity.
(5) Detecting and judging the purified soil, and backfilling after the purified soil is qualified; the unqualified pulp is returned to the pulping tank for further treatment.
The results of the ex-situ remediation of mercury contaminated soil are shown in table 2.
Table 2 results of the treatment of ex-situ remediation of mercury contaminated soil in example 2.
The technical principle of the invention is as follows:
placing heavy metal-containing soil in NaCl electrolyte, stirring to make particles keep suspension state, making anode be pretreated graphite material and cathode be stainless steel or alloy aluminium, when the direct current is passed between the electrodes, making different reactions occur between cathode and anode, and in the anode, producing oxidant (ClO) in the solution-) And further dissolving mercury; at the cathode, mercury is reduced quickly; hg ions can form Hg complex ions in the chloride solution, so that the chloride solution has high solubility; the Hg does not react with the electrode material, and drops form on the cathode surface, and sinks to the bottom of the electrolytic cell in the form of mercurous chloride which is insoluble and then recovered.
The reaction formula is as follows:
and (3) anode reaction: hg +2ClO-+4Cl-+2H2O=Cl2+HgCl4 2-+4OH-
And (3) cathode reaction: HgCl4 2-+2e=Hg+4Cl-
Hg+Hg2++2Cl-=Hg2Cl2↓
Claims (1)
1. A method for ex-situ remediation of mercury contaminated soil is characterized by comprising the following steps:
(1) after being excavated in layers, conveyed and metered, mercury-containing soil enters a pre-soaking reactor, and is subjected to pre-soaking reaction and filter pressing for solid-liquid separation, so that filter cakes and filtrate are separated; the pre-soaking reaction liquid is a mixed liquid of sodium chloride and hydrochloric acid, wherein the concentration of the sodium chloride is 20-30g/L, and the concentration of the hydrochloric acid is 10-15 g/L; the solid-to-solid mass ratio of the presoaking reaction liquid is as follows: 5-7: 1; the reaction time is 120-180 min; the stirring speed is as follows: 120-150 rpm;
(2) the filtrate generated by solid-liquid separation in the step (1) is subjected to mercury removal to generate a mercury sulfide product, and the mercury-removed liquid returns to the pre-soaking reactor; the mercury removing agent is sodium sulfide, and the adding amount is 3-5% of the excessive reaction amount;
(3) filter cakes generated by solid-liquid separation in the step (1) enter a slurrying tank for slurrying, then enter an ore pulp electrolytic tank, air is changed into compressed air through an air compressor and enters the ore pulp electrolytic tank, and meanwhile, ore pulp is stirred between a cathode and an anode through a stirrer to keep the ore pulp uniform; the liquid-solid mass ratio of the filter cake entering a slurrying tank for slurrying is 8-10: 1; the compression multiple of the compressed air is 15-20 times; the stirring speed is 20-30 rpm;
(4) after the ore pulp electrolytic cell is prepared in the step (3), after the ore pulp is homogenized by compressed air and stirring, the ore pulp is prevented from being layered, then direct current is introduced into the cathode and the anode of the ore pulp electrolytic cell, and the ore pulp electrolysis condition is as follows: the anode is a graphite polar plate, and the cathode is a stainless steel or aluminum plate; the effective area ratio of the anode to the cathode is as follows: 1.5-2: 1; the anode current density was: 400-500A/m2And the cathode current density is: 800-1000A/m2(ii) a The catholyte comprises mixed solution of sodium chloride and hydrochloric acid, wherein the concentration of sodium chloride is 20-30g/L, and the concentration of hydrochloric acid is 10-15 g/L; the component of the anolyte is sodium chloride solution, and the concentration of the sodium chloride solution is 50-60 g/L; the anode diaphragm bag is made of polypropylene or polytetrafluoroethylene materials, the electrolysis time is three to four electrolysis cycles, and each electrolysis cycle is 3 to 6 hours; after the pulp electrolysis, the mercurous chloride discharged from the bottom of the tank is dissolved in the solutionPartially flowing out, and treating to obtain a product; the slurry flows out from the side surface of the ore pulp electrolytic tank, the slurry is subjected to solid-liquid separation through filter pressing, and the leachate enters a catholyte storage tank and then enters a replenishment head tank through conveying; the solution in the elevated tank enters the ore pulp electrolytic tank under the action of gravity; carrying out filter pressing on the slurry twice, wherein a filter cake obtained after the first filter pressing stays in a filter press and needs to be washed for 3-5 times, and when the pH value of a filtrate is within the range of 6-8, carrying out filter pressing again;
(5) detecting and judging the purified soil, and backfilling after the purified soil is qualified; the unqualified pulp is returned to the pulping tank for further treatment.
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| CN115213214B (en) * | 2022-05-31 | 2024-05-28 | 江苏隆昌化工有限公司 | Cadmium-reducing and mercury-reducing material for producing polluted farmland of cloud precious plateau by using phosphogypsum and pyrite as resources |
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| US5244492A (en) * | 1992-06-26 | 1993-09-14 | Ppg Industries, Inc. | Process for recovery of metallic mercury from contaminated mercury-containing soil |
| CN1104265A (en) * | 1993-12-24 | 1995-06-28 | 化学工业部天津化工研究院 | Suspension electrolyte technology for copper mine |
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