CN112642850A - Remediation method for antagonistic heavy metal contaminated soil - Google Patents
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Abstract
The invention provides a remediation method for antagonistic heavy metal contaminated soil. The restoration method utilizes the sequential addition of the activated phosphorus modified hydrothermal carbon and the activated iron modified hydrothermal carbon, reduces the antagonism of the coexistence of three heavy metals of cadmium, lead and arsenic, and reduces the leaching state content of the cadmium, lead and arsenic by more than 90 percent aiming at the condition that the cadmium, lead and arsenic can simultaneously reach the TCLP leaching state content. The repairing method, the repairing process and the adopted materials are green and pollution-free, firstly the source is the biomass material, secondly in the material preparation and modification processes, the used reagents are mostly non-toxic and do not contain ions polluting the soil, and finally the usage amount of the stabilizing agent is small and neutral, and has no obvious influence on the pH value and the physical property of the soil.
Description
Technical Field
The invention belongs to the technical field of heavy metal contaminated soil treatment, and particularly relates to a remediation method for antagonistic heavy metal contaminated soil.
Background
At present, the heavy metal pollution condition of soil is not optimistic, and the problem of multiple heavy metal combined pollution exists. Particularly, the over-standard position point of heavy metal in the mining area soil is As high As 33.4%, the main elements polluted by the heavy metal soil are Cd, Pb and As, and the heavy metal pollution of the soil around the non-ferrous metal mining area is more serious.
The stabilization and remediation are one of the main technologies for soil heavy metal pollution remediation, and the stabilization material is the core of the stabilization and remediation technology. The stabilizing materials comprise clay materials, phosphorus-containing materials, organic materials and the like, and promote the migration of pollutants in soil and reduce environmental risks through the effects of adsorption, surface complexation, oxidation reduction, precipitation, coprecipitation and the like of the stabilizing materials on heavy metals. However, on the one hand, the remediation effect of heavy metal contaminated soil by the stabilizing material is different due to the influence of various factors in the soil; on the other hand, compared with single pollution, the heavy metal compound polluted soil has interaction among elements or compounds, and the interaction can influence the remediation of the polluted soil.
The existing research mainly improves the stabilizing effect on the heavy metal in the soil by compounding various stabilizing agents, but most of stabilizing agents with better effect have chemical toxicity, so that the secondary pollution to the soil is easily caused by improper application. In addition, most stabilizing agents aim at single heavy metal contaminated soil or soil contaminated by several heavy metals with similar remediation principles, and an effective remediation method is still lacked for heavy metal composite contaminated soil with antagonistic factors (such as cadmium, lead and arsenic).
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. Therefore, the invention provides a remediation method for antagonistic heavy metal contaminated soil, which can effectively treat heavy metal contaminated soil with antagonistic factors and reduce the influence of antagonism.
A remediation method for antagonistic heavy metal contaminated soil comprises the following steps:
s1: adding activated phosphorus modified hydrothermal carbon into antagonistic heavy metal contaminated soil, and standing for the first time after ploughing;
s2: adding activated iron modified hydrothermal carbon into the soil treated in the step S1, and standing for the second time after ploughing;
the antagonistic heavy metal contaminated soil comprises soil compositely contaminated by cadmium, lead and arsenic.
Meanwhile, in the soil compositely polluted by cadmium, lead and arsenic, compared with the soil singly polluted, the soil has different physical and chemical properties and characteristics of pollutants, and the complexity of soil pollution is increased. In general, interactions between complex contaminants occur, manifested as antagonism, additivity and synergy. Antagonism refers to the presence of one contaminant that inhibits the absorption of another contaminant and its biological effects. During the transportation and absorption of various pollutants in animals and plants, the binding sites on the carrier are subjected to mutual competition, so that the absorption of a certain pollutant is influenced. When cadmium and lead coexist, lead can capture the adsorption sites of cadmium in soil, increase the activity of cadmium and improve the bioavailability of cadmium in soil. Under the coexistence condition of lead in soil, the absorption of arsenic by plants is obviously reduced.
The fixation of heavy metals in soil is greatly influenced by pH, and as pH decreases, different heavy metals show different mobility characteristics under the influence of pH. The solubility of cadmium in the range of 3-8 is reduced along with the increase of pH; lead solubility is increased after pH is higher than 6, and As has stronger solubility in alkaline solution. The above-mentioned influence makes it difficult to fix three heavy metals simultaneously.
The phosphate passivator comprises solubility (phosphoric acid, monopotassium phosphate, monocalcium phosphate and the like) and insolubility (phosphogypsum, phosphate rock, hydroxyapatite and the like). Whether the insoluble phosphate can well passivate heavy metals in soil is mainly limited by the pH value of the soil. At pH 5, lead is deactivated relatively quickly, mainly because of the formation of Pb at this pH5(PO4)3The OH speed is very fast. Soluble phosphates, when added to soil, lower the pH of the soil and thereby increase the leaching of other heavy metals such as arsenic. Phosphorus and arsenic are elements of the same group, and they are similar in nature and exert antagonistic action, resulting in PO4 3-With AsO4 3-Formation of competitive adsorption, PO4 3-To replace AsO in soil4 3-Thereby releasing arsenic and enhancing its mobility.
In the activated iron modified hydrothermal carbon, iron ions are attached to pores of the hydrothermal carbon and can be coprecipitated with heavy metals in soil, so that the stabilizing effect on the heavy metals is improved.
The activated phosphorus modified hydrothermal carbon can improve the hydrophilicity of the hydrothermal carbon, change the specific surface area and active functional groups of the hydrothermal carbon, and further improve the stabilizing effect on heavy metals (particularly Pb ions).
According to an embodiment of the invention, in step S1, the activated phosphorus modified hydrothermal carbon is added in an amount of 3 to 7 wt%.
According to an embodiment of the invention, in step S2, the activated iron-modified hydrothermal carbon is added in an amount of 3 to 7 wt%.
According to one embodiment of the invention, the addition mass ratio of the activated phosphorus modified hydrothermal carbon to the activated iron modified hydrothermal carbon is (0.5-1.5): 1.
according to a preferred embodiment of the present invention, the addition mass ratio of the activated phosphorus-modified hydrothermal carbon to the activated iron-modified hydrothermal carbon is 1: 1.
according to one embodiment of the invention, the preparation method of the activated phosphorus modified hydrothermal carbon comprises the following steps: and uniformly mixing the activated hydrothermal carbon with the phosphorus source solution, heating, filtering, and pyrolyzing filter residues to obtain the activated phosphorus modified hydrothermal carbon.
According to one embodiment of the invention, the phosphorus source solution is a hydroxyapatite suspension.
According to one embodiment of the invention, the preparation method of the activated iron modified hydrothermal carbon comprises the following steps: and uniformly mixing the activated hydrothermal carbon with the ferric salt solution, adjusting the pH value, filtering, and pyrolyzing filter residues to obtain the activated iron modified hydrothermal carbon.
According to one embodiment of the present invention, the iron salt solution is a mixed solution of a ferrous salt and a ferric salt.
According to one embodiment of the invention, the preparation method of the activated hydrothermal carbon comprises the following steps: adding a biomass raw material into a high-pressure reaction kettle for reaction, drying, grinding and sieving by a 60-mesh sieve to obtain hydrothermal carbon, adding the hydrothermal carbon into an alkali solution, soaking at normal temperature, and pyrolyzing to obtain the activated hydrothermal carbon. Wherein the pyrolysis temperature is 300 ℃ and the time is 1 h.
Wherein the biomass material comprises rice straw, palm leaf, pine log and bamboo, preferably palm leaf.
And (3) carrying out reaction in a high-pressure reaction kettle at the temperature of 140-200 ℃ for 4-8 h.
The reaction is carried out in a high-pressure reaction kettle, the reaction temperature is preferably 180 ℃, and the reaction time is 6 hours.
The hydrothermal carbon is added into the alkali solution, so that the basic groups such as hydroxyl, amino and the like of the hydrothermal carbon can be increased, and more adsorption sites are provided; the alkali solution has strong corrosivity on the hydrothermal carbon, so that fragments among gaps of the hydrothermal carbon and hole walls are corroded, inner pore passages of the hydrothermal carbon are dredged to form micropores, and the specific surface area and the pore diameter of the micropores are increased.
According to one embodiment of the invention, the alkali solution is a NaOH solution or a KOH solution.
According to an embodiment of the invention, the time for the first standing is 12-36 h.
According to an embodiment of the invention, the time of the second standing is 36-60 h.
The remediation method for the soil polluted by the antagonistic heavy metal at least has the following technical effects:
the restoration method utilizes the sequential addition of the activated phosphorus modified hydrothermal carbon and the activated iron modified hydrothermal carbon, reduces the antagonism of the coexistence of three heavy metals of cadmium, lead and arsenic, and reduces the leaching state content of the cadmium, lead and arsenic by more than 90 percent aiming at the condition that the cadmium, lead and arsenic can simultaneously reach the TCLP leaching state content.
The repairing method, the repairing process and the adopted materials are green and pollution-free, firstly, the materials are biomass materials, secondly, in the processes of preparing and modifying the materials, most of used reagents are non-toxic and do not contain ions polluting soil, and finally, the usage amount of a stabilizing agent is small and neutral, and the pH and the physical properties of the soil are not greatly influenced.
Drawings
FIG. 1 XRD pattern of ordinary hydrothermal carbon prepared in example 1.
FIG. 2 is a microscopic morphology image of the activated hydrothermal carbon prepared in example 2 by a scanning electron microscope.
FIG. 3 is a scanning electron microscope microscopic morphology image of the activated iron modified hydrothermal carbon prepared in example 3.
FIG. 4 XRD pattern of activated iron modified hydrothermal carbon prepared in example 3.
FIG. 5 is a scanning electron microscope microscopic morphology of the activated phosphorus modified hydrothermal carbon prepared in example 4.
FIG. 6 XRD pattern of activated phosphorus modified hydrothermal carbon prepared in example 4.
FIG. 7 shows the Fourier transform infrared spectroscopy test results for the activated hydrothermal carbon prepared in example 2.
FIG. 8 is a Fourier transform infrared spectroscopy test of the activated iron modified hydrothermal carbon prepared in example 3.
FIG. 9 is a Fourier transform infrared spectroscopy test of the activated phosphorus-modified hydrothermal carbon prepared in example 4.
Detailed Description
The following are specific examples of the present invention, and the technical solutions of the present invention will be further described with reference to the examples, but the present invention is not limited to the examples.
Example 1
The embodiment prepares the common hydrothermal carbon, and the specific preparation method comprises the following steps: adding the biomass raw material into a high-pressure reaction kettle for reaction, and drying to obtain the biomass material. Wherein the biomass material is palm leaves.
And (3) carrying out reaction in a high-pressure reaction kettle at the temperature of 140-200 ℃ for 4-8 h.
The X-ray diffraction results of the ordinary hydrothermal carbon prepared in this example are shown in FIG. 1.
Adding hydrothermal carbon under different preparation conditions into the soil TCLP leaching liquor, fully mixing uniformly, placing in a constant temperature shaking table for shake culture for 24h, setting the temperature at 25 ℃ and the rotating speed at 180 r/min. Filtering, and collecting supernatant for chemical detection.
The stabilization rates of the common hydrothermal carbon prepared under different preparation temperatures and conditions on cadmium, lead and arsenic were tested. The results are shown in Table 1.
TABLE 1 detection results of cadmium, lead and arsenic
| Cadmium stabilization Rate/% | Lead stabilization rate/%) | Arsenic stabilization Rate/%) | |
| 160℃，6h | 2.06％ | -13.85％ | -9.94％ |
| 180℃，4h | 1.37％ | -1.52％ | -27.24％ |
| 180℃，6h | 13.01％ | -1.52％ | 15.79％ |
| 180℃，8h | -8.22％ | -6.76％ | -42％ |
| 200℃，8h | 8.22％ | -13.85％ | 0.03％ |
As can be seen from Table 1, the conditions at 180 ℃ for 6 hours were the best when the reaction was carried out in the autoclave.
Example 2
The embodiment prepares the activated hydrothermal carbon, and the preparation method comprises the following steps: the common hydrothermal carbon prepared in the embodiment 1 at 180 ℃ for 6h is added into the alkali solution, and the activated hydrothermal carbon is obtained after normal temperature dipping and pyrolysis. Wherein the pyrolysis temperature is 300 ℃ and the time is 1 h.
Wherein the alkali solution is KOH solution with the concentration of 1mol/L, and the ratio of the common hydrothermal carbon to the alkali solution is 1:2(g: mL). The micro-morphology of the common hydrothermal carbon prepared in this example is shown in fig. 2, and it can be seen from fig. 2 that the surface of the common hydrothermal carbon is relatively smooth and flat.
Example 3
The embodiment prepares the activated iron modified hydrothermal carbon, and the preparation method comprises the following steps: mixing the activated hydrothermal carbon prepared in the previous step in a ratio of 1: 5 (g: mL) and 0.5 mol/L1: 1 molar ratio of Fe2+/Fe3+Mixing the mixed iron solution, stirring thoroughly for 30min, adjusting pH of the system to 10, measuring pH after stirring thoroughly for 30min, adjusting pH to 10 again when pH changes, filtering, oven drying, and cracking at 300 deg.C for 1 h.
The micro-morphology of the activated iron-modified hydrothermal carbon prepared in this example is shown in fig. 3, and it can be seen from fig. 3 that the surface of the activated iron-modified hydrothermal carbon is rough and granular substances are attached.
The X-ray diffraction results of the activated iron modified hydrothermal carbon prepared in this example are shown in FIG. 4, and magnetite can be seen from FIG. 4, indicating the success of iron modification.
Example 4
The embodiment prepares the activated phosphorus modified hydrothermal carbon, and the preparation method comprises the following steps: and (3) uniformly mixing the activated hydrothermal carbon prepared in the previous step with a phosphorus source solution, heating, filtering, and pyrolyzing filter residues to obtain the activated phosphorus modified hydrothermal carbon.
The phosphorus source solution is a hydroxyapatite aqueous solution, and the hydroxyapatite aqueous solution is prepared by mixing 12g of micron-sized hydroxyapatite with 2000mL of distilled water, and heating for 1 h.
The micro-morphology of the activated phosphorus-modified hydrothermal carbon prepared in this example is shown in fig. 5, and it can be seen from fig. 5 that the surface of the activated phosphorus-modified hydrothermal carbon is rough and spherical particles are attached to the surface.
The X-ray diffraction results of the activated iron-modified hydrothermal carbon prepared in this example are shown in FIG. 6, and the apatite component is seen from FIG. 6, indicating the success of phosphorus modification.
Example 5
The activated iron-phosphorus modified hydrothermal carbon is prepared according to the embodiment, and the preparation method comprises the steps of firstly preparing the activated iron modified hydrothermal carbon according to the steps, and then treating the activated iron modified hydrothermal carbon according to the preparation method of the activated phosphorus modified hydrothermal carbon to obtain the activated iron-phosphorus modified hydrothermal carbon.
Detection example 1
X-ray energy spectrum analysis was performed on ordinary hydrothermal carbon, activated iron-modified hydrothermal carbon, and activated phosphorus-modified hydrothermal carbon prepared in example 1, example 3, and example 4. The results are shown in Table 2.
TABLE 2X-ray spectral analysis results
As can be seen from the results in Table 2, the contents of Cl, K, Mn and Fe in the activated iron modified hydrothermal carbon are obviously increased, and the contents of Mg, Ca, K and P in the activated phosphorus modified hydrothermal carbon are obviously increased.
Detection example 2
The activated hydrothermal carbon, the activated iron-modified hydrothermal carbon, the activated phosphorus-modified hydrothermal carbon, and the activated iron-phosphorus-modified hydrothermal carbon prepared in examples 2 to 5 were tested for their stabilization rates for cadmium, lead, and arsenic. The results are shown in Table 3.
TABLE 3 detection results of cadmium, lead and arsenic
| Hydrothermal charcoal type | Cadmium stabilization Rate/% | Lead stabilization rate/%) | Arsenic stabilization Rate/%) |
| Activated hydrothermal charcoal | 57.63 | 91.32 | 58.45 |
| Activated iron modified hydrothermal carbon | 45.10 | 99.14 | 96.79 |
| Activated phosphorus modified hydrothermal carbon | 97.21 | 99.94 | 71.32 |
| Activated iron-phosphorus modification | 91.62 | 99.96 | 98.34 |
Detection example 3
The hydrothermal carbon prepared in the examples 1 to 4 is respectively added into different parts of antagonistic heavy metal contaminated soil with the same pollution condition, and the antagonistic heavy metal contaminated soil is soil compositely contaminated by cadmium, lead and arsenic. The method comprises the following specific steps:
s1: adding the activated phosphorus modified hydrothermal carbon prepared in the example 2 into antagonistic heavy metal contaminated soil, and standing for the first time after ploughing;
s2: adding the activated iron modified hydrothermal carbon prepared in example 3 to the soil treated in step S1, turning, and standing for the second time;
wherein, the time of the first standing is 24 hours, and the time of the second standing is 48 hours.
After standing, the soil was air-dried, sampled from the soil, ground, subjected to TCLP leaching, and tested for the available states of Cd, Pb, As in the soil, and the results are shown in table 4.
TABLE 4
The results in Table 4 show that the stabilization effect of the activated phosphorus modified hydrothermal carbon added first and then the activated iron modified hydrothermal carbon on Cd, Pb and As in the soil is better than that of the activated iron-phosphorus modified hydrothermal carbon, so that the effective states of Cd, Pb and As in the soil are respectively reduced by 35.14mg/kg, 762.2mg/kg and 4.79mg/kg, and are reduced by 20.37%, 82.56% and 39.04%.
In addition, the activated hydrothermal carbon prepared in example 2, the activated iron-modified hydrothermal carbon prepared in example 3, and the activated phosphorus-modified hydrothermal carbon prepared in example 4 were examined by Fourier Transform Infrared Spectrometer (FTIR Spectrometer for short), as shown in fig. 7, fig. 8, and fig. 9, respectively. Fig. 7 is the activated hydrothermal carbon prepared in example 2, fig. 8 is the activated iron-modified hydrothermal carbon prepared in example 3, and fig. 9 is the activated phosphorus-modified hydrothermal carbon prepared in example 4. Similar absorption peaks appear before and after modification of the hydrothermal carbon, mainly comprising 3354.20, 2923.01, 1607.72-1455.38, 1058.04 and 666.86cm-1。
Wherein 3354.20cm-1Is associated with hydroxyl (-OH) stretching vibration peak, and the hydroxyl is mainly derived from carbohydrate in biomassThe peak intensity and peak intensity of the compound are reduced after modification, which shows that hydroxyl groups are reduced by iron modification and phosphorus modification.
2923.01cm-1The peak intensity is reduced after modification due to the stretching vibration peak of carboxyl (-OH), which indicates that carboxyl groups are reduced by iron modification and phosphorus modification.
1607.72-1455.38cm-1The peak intensity is reduced after modification, which shows that benzene groups are reduced by iron modification and phosphorus modification.
1058.04cm-1The peak intensity of iron modification is reduced when the peak intensity of carbonyl (-CO) stretching vibration is detected, which shows that the carbonyl is reduced by the iron modification, and the carbonyl is increased by the phosphorus modification.
At 666.86, 617.62cm-1The peak is an aliphatic C-Cl stretching vibration peak, and the peak strength is increased after modification, which indicates that the substitution reaction of the organic halide occurs.
The present invention has been described in detail with reference to the embodiments, but the present invention is not limited to the embodiments described above, and various changes can be made within the knowledge of those skilled in the art without departing from the gist of the present invention.
Claims (10)
1. The remediation method for the heavy metal polluted soil is characterized by comprising the following steps:
s1: adding activated phosphorus modified hydrothermal carbon into antagonistic heavy metal contaminated soil, and standing for the first time after ploughing;
s2: adding activated iron modified hydrothermal carbon into the soil treated in the step S1, and standing for the second time after ploughing;
the antagonistic heavy metal contaminated soil comprises soil compositely contaminated by cadmium, lead and arsenic.
2. The repair method according to claim 1, wherein in step S1, the activated phosphorus-modified hydrothermal carbon is added in an amount of 3 to 7 wt%.
3. The repair method according to claim 1, wherein in step S2, the activated iron-modified hydrothermal carbon is added in an amount of 3 to 7 wt%.
4. The repair method according to claim 1, wherein the addition mass ratio of the activated phosphorus-modified hydrothermal carbon to the activated iron-modified hydrothermal carbon is (0.5-1.5): 1.
5. the repair method according to claim 1, wherein the activated phosphorus-modified hydrothermal carbon is prepared by the following method: and uniformly mixing the activated hydrothermal carbon with the phosphorus source solution, heating, filtering, and pyrolyzing filter residues to obtain the activated phosphorus modified hydrothermal carbon.
6. The repair method according to claim 5, wherein the phosphorus source solution is a hydroxyapatite suspension.
7. The repair method according to claim 1, wherein the activated iron-modified hydrothermal carbon is prepared by the following method: and uniformly mixing the activated hydrothermal carbon with the ferric salt solution, adjusting the pH value, filtering, and pyrolyzing filter residues to obtain the activated iron modified hydrothermal carbon.
8. The method for repairing according to claim 5 or 7, wherein the activated hydrothermal carbon is prepared by: adding a biomass raw material into a high-pressure reaction kettle for reaction, drying, grinding and sieving by a 60-mesh sieve to obtain hydrothermal carbon, adding the hydrothermal carbon into an alkali solution, soaking at normal temperature, and pyrolyzing to obtain the activated hydrothermal carbon.
9. The repair method according to claim 1, wherein the first standing time is 12 to 36 hours.
10. The repair method according to claim 1, wherein the time for the second standing is 36 to 60 hours.
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