CN106975655B - In-situ chemical oxidation remediation method for organic contaminated site soil based on iron cycle regulation - Google Patents
In-situ chemical oxidation remediation method for organic contaminated site soil based on iron cycle regulation Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
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Abstract
The invention relates to an in-situ chemical oxidation remediation method for organic contaminated site soil based on iron cycle regulation. The method comprises the following steps: adding a mixed solution of natural organic micromolecules and hydrogen peroxide into the soil of the organic pollution field to be repaired, activating naturally-existing iron minerals in the soil by using the natural organic micromolecules to serve as an effective iron source for decomposing the hydrogen peroxide, and efficiently decomposing the hydrogen peroxide into hydroxyl free radicals to realize the in-situ chemical oxidation repair of the soil of the organic pollution field. The method utilizes natural organic micromolecules to activate the naturally-existing iron minerals in the soil, solves the problems that ferrous ions need to be additionally added in the traditional hydrogen peroxide chemical oxidation technology and mass transfer between hydroxyl radicals generated by decomposition of hydrogen peroxide and soil organic pollutants is caused by direct contact, and has the advantages of high efficiency, no selectivity, cost saving, environmental friendliness, no secondary pollution and the like when being used for in-situ chemical oxidation remediation of the soil polluted by the organic matters.
Description
Technical Field
The invention belongs to the field of environmental chemistry, and particularly relates to a method for controlling and repairing organic pollutants in soil, which is suitable for repairing organic polluted soil in the fields of printing and dyeing, industry, agriculture and the like.
Background
Soil is an important natural resource on earth and is the basis on which life depends to survive and develop. With the rapid growth of population and the rapid development of industry and agriculture in China, a large amount of harmful wastewater, solid waste and the like are promoted to be continuously discharged into the nature, and the problem of soil pollution is increasingly highlighted. Among them, the organic contaminated soil has many kinds of pollutants, and most of them have high toxicity and are difficult to degrade under natural conditions, which poses a significant threat to the good operation of the whole ecological environment.
The Fenton technology has the most remarkable characteristic of generating hydroxyl free radicals (. OH) with strong oxidizing property, and is suitable for treating and repairing organic contaminated soil. In the prior art, the Fenton technology is applied to actual soil remediation, and generally additional ferrous ions are needed as an oxidant activator, but the additional ferrous ions increase the content of iron in water and soil to form secondary pollution, and the ferrous ions are difficult to recycle, so that resource waste is caused. In addition, in the soil, the reaction of the added ferrous ions and hydrogen peroxide needs to be carried out under the condition of lower pH value (2-3.5). However, by adjusting the pH of the soil to between 2 and 3.5, the soil will be severely damaged and cause more serious pollution.
Disclosure of Invention
The invention aims to solve the technical problem of providing an in-situ chemical oxidation remediation method for organic contaminated site soil based on iron cycle regulation and control, aiming at the defects of the oxidation remediation method requiring the addition of ferrous ions. The method is used for restoring the soil in the organic polluted site, has good restoration effect, does not need to add ferrous ions, does not need to adjust the pH value, and does not generate secondary pollution.
The technical scheme adopted by the invention for solving the problems is as follows:
an in-situ chemical oxidation remediation method for organic contaminated site soil based on iron cycle regulation and control is characterized by comprising the following steps: adding a mixed solution of natural organic micromolecules and hydrogen peroxide into the soil of the organic pollution field to be repaired, activating naturally-existing iron minerals in the soil by using the natural organic micromolecules to serve as an effective iron source for decomposing the hydrogen peroxide, and efficiently decomposing the hydrogen peroxide into hydroxyl free radicals to carry out in-situ chemical oxidation repair on the soil of the organic pollution field.
According to the scheme, the concentration of the natural organic micromolecules in the mixed solution is 2-50 mmol/L; the concentration of the hydrogen peroxide in the mixed solution is 100-1000 mmol/L.
According to the scheme, the natural organic small molecular substance is one of gallic acid, ascorbic acid, protocatechuic acid, oxalic acid and tartaric acid.
According to the scheme, the natural organic micromolecule substance is selected from one of gallic acid, ascorbic acid, protocatechuic acid, oxalic acid and tartaric acid and a mixture thereof. According to the scheme, after the organic contaminated site soil is sampled, the uniform soil sample is formed through freeze-drying, smashing and grinding.
According to the scheme, the organic pollutants comprise but are not limited to o-chloronitrobenzene and p-chloronitrobenzene.
According to the scheme, the mixed solution of natural organic micromolecules and hydrogen peroxide is added to repair the soil of the organic contaminated site, and the system is not stirred.
According to the scheme, the mixed solution of the natural organic micromolecules and the hydrogen peroxide is added into the soil for repairing without adjusting the pH value in the system.
The technical principle of the invention is as follows:
the soil generally contains natural iron-containing minerals (oxides and hydroxides), and the interfacial action and the surface redox reaction of the iron-containing minerals play important roles in the environmental geochemical process. The existing valence states of iron in minerals are mainly two types: ferrous iron and ferric iron. The Fe (III)/Fe (II) cycle plays an important role in the geochemical and biogeochemical evolution process of the surface elements.
The natural organic small molecules influence the migration, transformation, sedimentation and bioavailability of metal ions and organic pollutants in soil in natural environment. The form and the content of iron on the surface interface of the iron ore can be adjusted by utilizing natural organic micromolecules, ferrous iron on the surface interface of the iron ore is continuously generated in situ by coordinating or reducing iron minerals in soil and underground water, and then the ferrous iron with high activity reacts with hydrogen peroxide to generate hydroxyl free radicals with strong oxidizing property, so that the aim of mineralizing organic pollutants in the soil without selectivity is fulfilled. The problem that ferrous ions need to be additionally added in the traditional chemical oxidation technology of hydrogen peroxide is solved, the mass transfer problem between the hydroxyl radicals generated by the decomposition of the hydrogen peroxide and the direct contact of soil organic pollutants is solved, the pH application range is wide, the pH value does not need to be adjusted, and the hydrogen peroxide has a good decomposition effect under the natural pH value.
The natural organic micromolecules generally have a reduction effect, can promote Fe (III)/Fe (II) circulation in soil, enhance the capability of iron minerals for activating oxidants, lead hydrogen peroxide to be continuously decomposed to generate hydroxyl free radicals, and achieve the purpose of utilizing the iron minerals to repair the organic polluted soil in situ. In the process of utilizing natural organic micromolecules to regulate and control iron circulation in-situ chemical oxidation to repair organic polluted soil, the natural organic micromolecules are also oxidized and degraded, and the risk of secondary pollution is further reduced.
The invention has the advantages that:
1. the invention uses natural organic micromolecules to regulate and control the iron circulation in the soil, regulates the content or concentration of low-valence Fe (II) on the surface interface of iron minerals in the soil, can improve the decomposition efficiency of hydrogen peroxide, generates more hydroxyl free radicals and efficiently removes organic pollutants. An additional iron compound is not required to be introduced, so that resources are saved and secondary pollution is reduced.
2. The natural organic micromolecules are generally simple in structure, high in natural content, widely existing in the environment, cheap, easy to obtain and environment-friendly, and can be degraded along with pollutants in the oxidation repair process without causing secondary pollution.
3. The reaction conditions are mild, the reaction can be carried out quickly at normal temperature and normal pressure, complex devices are not needed, the operation is simple, no danger exists, and no professional is needed for operation.
4. The method does not need to adjust the pH value of the environment, and the natural organic micromolecules are used in the chemical oxidation remediation process of the soil, so that the change of the pH value of the soil system is small, and the trouble can not be brought to the actual remediation process. In the repair process, natural organic small molecules are also oxidized and degraded, so that the risk of secondary pollution is further reduced.
5. A small amount of water is introduced in the reaction process, so that a good contaminated soil remediation effect can be achieved, and convenience is provided for in-situ remediation of actual contaminated soil.
Drawings
FIG. 1 is a diagram showing the effect of the method of the present invention in remediation of chloronitrobenzene in soil contaminated with chloronitrobenzene;
FIG. 2 is a graph showing the effect of the method of the present invention on remediation of chloronitrobenzene in soil contaminated with chloronitrobenzene;
FIG. 3 is a graph showing the effect of the method of the present invention on remediation of chloronitrobenzene in soil contaminated with chloronitrobenzene at different ascorbic acid concentrations;
FIG. 4 is a graph showing the effect of the method of the present invention on the remediation of chloronitrobenzene in soil contaminated with chloronitrobenzene at different ascorbic acid concentrations;
FIG. 5 is a graph showing the effect of the method of the present invention on remediation of chloronitrobenzene in soil contaminated with chloronitrobenzene at different concentrations of hydrogen peroxide;
FIG. 6 is a graph showing the effect of the method of the present invention on the remediation of chloronitrobenzene in soil contaminated with chloronitrobenzene at different concentrations of hydrogen peroxide;
FIG. 7 is a graph showing the effect of hydrogen peroxide of different concentrations on remediation of o-chloronitrobenzene in soil in a chloronitrobenzene contaminated site;
FIG. 8 is a graph showing the effect of hydrogen peroxide of different concentrations on remediation of chloronitrobenzene contaminated site soil;
FIG. 9 is a graph showing the effect of the method of the present invention on remediation of chloronitrobenzene in soil in a chloronitrobenzene contaminated site at different contaminated soil dosing amounts;
FIG. 10 is a graph showing the effect of the method of the present invention on the remediation of chloronitrobenzene in soil in a chloronitrobenzene contaminated site at different contaminated soil dosing amounts;
FIG. 11 is a graph showing the effect of the method of the present invention on remediation of chloronitrobenzene in soil contaminated with chloronitrobenzene under different water source conditions;
FIG. 12 is a graph showing the effect of the method of the present invention on remediation of chloronitrobenzene in soil contaminated with chloronitrobenzene under different water source conditions.
FIG. 13 is a graph showing the effect of the method of the present invention on the remediation of chloronitrobenzene from chloronitrobenzene contaminated site soil under different natural organic small molecule conditions;
FIG. 14 is a graph showing the effect of the method of the present invention on the remediation of chloronitrobenzene in soil contaminated with chloronitrobenzene under different natural organic small molecule conditions.
Detailed Description
The following detailed description of the present invention is provided by way of specific embodiments, which are provided for illustration purposes and are not intended to limit the invention.
Example 1 remediation of Chloronitrobenzene-contaminated site soil
The organic contaminated site soil is taken from a chloronitrobenzene contaminated site of a certain abandoned chemical plant, and after sampling, the contaminated soil is freeze-dried, smashed and ground into a uniform soil sample. And determining main organic pollutants in the polluted soil to be o-chloronitrobenzene and p-chloronitrobenzene through mass spectrum detection.
Aiming at the remediation of the soil of the chloronitrobenzene polluted site, 1mL of mixed solution of ascorbic acid and hydrogen peroxide is added into 1g of soil, so that the concentrations of the ascorbic acid and the hydrogen peroxide are respectively 10mmol/L and 200mmol/L, the pH is not required to be adjusted additionally, and the mixture is kept stand. Meanwhile, the degradation conditions of o-chloronitrobenzene and p-chloronitrobenzene are respectively monitored by taking the control experiment of adding no ascorbic acid and hydrogen peroxide, adding only ascorbic acid or only hydrogen peroxide, and respectively setting the concentrations of the ascorbic acid and the hydrogen peroxide in the control experiment to be 10mmol/L and 200mmol/L, and the results are shown in a graph 1 and a graph 2. As shown in figure 1, after the reaction is carried out for 72 hours, the degradation rate of o-chloronitrobenzene in the soil reaches 93 percent. As shown in figure 2, the degradation rate of p-chloronitrobenzene in the soil reaches 90 percent after the reaction is carried out for 48 hours.
Example 2 remediation of chloronitrobenzene contaminated site soil at different ascorbic acid concentrations
The organic contaminated site soil is taken from a chloronitrobenzene contaminated site of a certain abandoned chemical plant, and after sampling, the contaminated soil is freeze-dried, smashed and ground into a uniform soil sample. And determining that the polluted soil contains o-chloronitrobenzene and p-chloronitrobenzene by mass spectrum detection.
Aiming at the remediation of the soil of the chloronitrobenzene polluted site, 1mL of mixed solution of ascorbic acid and hydrogen peroxide is added into 1g of soil, the concentration of the hydrogen peroxide is 200mmol/L, the concentration of the ascorbic acid is 2, 5, 10 and 20mmol/L respectively, the pH is not required to be adjusted additionally, the mixture is kept stand, the degradation conditions of o-chloronitrobenzene and p-chloronitrobenzene are monitored respectively, and the results are shown in a graph 3 and a graph 4. As shown in FIG. 3, the degradation rate of o-chloronitrobenzene is increased and then decreased along with the increase of the initial concentration of ascorbic acid, when the initial concentration of ascorbic acid is 10mmol/L, the removal effect of o-chloronitrobenzene is the best, and the degradation rate of o-chloronitrobenzene reaches 93% after the reaction is carried out for 72 hours. As shown in FIG. 4, the degradation rate of p-chloronitrobenzene is increased and then decreased along with the increase of the initial concentration of ascorbic acid, when the initial concentration of ascorbic acid is 10mmol/L, the removal effect of p-chloronitrobenzene is the best, and the degradation rate of p-chloronitrobenzene reaches 90 percent after reaction for 48 hours.
Example 3 remediation of chloronitrobenzene contaminated site soil at different Hydrogen peroxide concentrations
The organic contaminated site soil is taken from a chloronitrobenzene contaminated site of a certain abandoned chemical plant, and after sampling, the contaminated soil is freeze-dried, smashed and ground into a uniform soil sample. And determining that the polluted soil contains o-chloronitrobenzene and p-chloronitrobenzene by mass spectrum detection.
Aiming at the remediation of the soil of the chloronitrobenzene polluted site, 1mL of mixed solution of ascorbic acid and hydrogen peroxide is added into 1g of soil, the concentration of the ascorbic acid is 10mmol/L, the concentration of the hydrogen peroxide is respectively 100, 200, 500 and 1000mmol/L, and the mixture is kept stand without adjusting the pH value additionally. Meanwhile, the degradation conditions of o-chloronitrobenzene and p-chloronitrobenzene are respectively monitored by taking the test without adding ascorbic acid as a control test, and the results are shown in fig. 5, fig. 6, fig. 7 and fig. 8. As shown in FIG. 5, the degradation rate of o-chloronitrobenzene is increased and then decreased along with the increase of the initial concentration of hydrogen peroxide, when the initial concentration of hydrogen peroxide is 200mmol/L, the o-chloronitrobenzene has the best removal effect, and the degradation rate of o-chloronitrobenzene reaches 93 percent after the reaction is carried out for 72 hours. As shown in FIG. 6, the degradation rate of p-chloronitrobenzene is increased and then decreased along with the increase of the initial concentration of hydrogen peroxide, when the initial concentration of hydrogen peroxide is 200mmol/L, the removal effect of p-chloronitrobenzene is the best, and the degradation rate of p-chloronitrobenzene reaches 90% after reaction for 48 hours. As shown in fig. 7 and 8, even when the initial concentration of hydrogen peroxide is 1000mmol/L, the degradation effect of o-chloronitrobenzene and p-chloronitrobenzene is still poor without adding ascorbic acid, and the degradation rate of o-chloronitrobenzene reaches 14% after 72 hours of reaction, and the degradation rate of p-chloronitrobenzene reaches 17% after 48 hours of reaction.
Example 4 remediation of Chloronitrobenzene contaminated site soil at different soil dosing amounts
The organic contaminated site soil is taken from a chloronitrobenzene contaminated site of a certain abandoned chemical plant, and after sampling, the contaminated soil is freeze-dried, smashed and ground into a uniform soil sample. And determining that the polluted soil contains o-chloronitrobenzene and p-chloronitrobenzene by mass spectrum detection.
For the remediation of the soil in the chloronitrobenzene polluted site, 1mL of a mixed solution of ascorbic acid and hydrogen peroxide is added into 0.1 g of soil, 0.5 g of soil, 1g of soil, 1.5g of soil, 2g of soil and 2.5g of soil respectively, so that the concentration of the ascorbic acid is 10mmol/L and the concentration of the hydrogen peroxide is 200mmol/L, the pH is not required to be adjusted additionally, the mixture is kept stand, and the degradation conditions of o-chloronitrobenzene and p-chloronitrobenzene are monitored respectively, and the results are shown in fig. 9 and fig. 10. As shown in FIG. 9, the degradation rate of o-chloronitrobenzene decreases with the increase of the dosage of the contaminated soil, and when the dosage of the contaminated soil is 0.1 g/mL, 0.5 g/mL, the time required for the o-chloronitrobenzene in the contaminated soil to completely degrade is 4 hours, 20 hours, 72 hours and 108 hours, respectively. When the soil addition amount is 2 and 2.5g/mL respectively, the reaction is carried out for 108 hours, and the degradation rate of o-chloronitrobenzene in the polluted soil reaches 62 percent and 37 percent respectively. As shown in FIG. 10, the degradation rate of p-chloronitrobenzene decreases with the increase of the dosage of the contaminated soil, and when the dosage of the contaminated soil is 0.1, 0.5, 1, 1.5 and 2g/mL hour, respectively, the time required for completely degrading p-chloronitrobenzene in the contaminated soil is 1, 15, 48, 72 and 108 hours, respectively. When the soil adding amount is 2.5g/mL respectively, the reaction is carried out for 108 hours, and the degradation rate of o-chloronitrobenzene in the polluted soil reaches 58%.
Example 5 remediation of Chloronitrobenzene contaminated site soil under different Water Source conditions
The organic contaminated site soil is taken from a chloronitrobenzene contaminated site of a certain abandoned chemical plant, and after sampling, the contaminated soil is freeze-dried, smashed and ground into a uniform soil sample. And determining that the polluted soil contains o-chloronitrobenzene and p-chloronitrobenzene by mass spectrum detection.
For the remediation of the soil in the chloronitrobenzene polluted site, a mixed solution of ascorbic acid and hydrogen peroxide is prepared by distilled water and tap water respectively, 1mL of the mixed solution of ascorbic acid and hydrogen peroxide is added into 1g of the soil, the concentration of the ascorbic acid is 10mmol/L respectively, the concentration of the hydrogen peroxide is 200mmol/L, pH is not required to be adjusted additionally, the mixture is kept stand in a dark place, the degradation conditions of o-chloronitrobenzene and p-chloronitrobenzene are monitored respectively, and the results are shown in figures 11 and 12. As shown in FIG. 11, the removal effect of o-chloronitrobenzene is not affected by using distilled water and tap water to prepare a mixed solution of ascorbic acid and hydrogen peroxide, and the degradation rate of o-chloronitrobenzene reaches 93% after reaction for 72 hours. As shown in FIG. 12, the mixed solution of ascorbic acid and hydrogen peroxide prepared from distilled water and tap water has no influence on the removal effect of p-chloronitrobenzene, and the degradation rate of p-chloronitrobenzene reaches 93% after 48 hours of reaction.
Example 6 remediation of Chloronitrobenzene contaminated site soil with different Natural organic Small molecules
The organic contaminated site soil is taken from a chloronitrobenzene contaminated site of a certain abandoned chemical plant, and after sampling, the contaminated soil is mixed, freeze-dried and ground into a uniform soil sample. And determining that the polluted soil contains o-chloronitrobenzene and p-chloronitrobenzene by mass spectrum detection.
Aiming at the remediation of the soil of the chloronitrobenzene polluted site, 1mL of gallic acid, ascorbic acid, protocatechuic acid, oxalic acid, tartaric acid and hydrogen peroxide mixed solution is added into 1g of soil, so that the concentrations of the gallic acid, the ascorbic acid, the protocatechuic acid, the oxalic acid, the tartaric acid and the hydrogen peroxide are respectively 10mmol/L and 200mmol/L, the pH is not required to be adjusted additionally, the mixture is kept stand, the degradation conditions of the o-chloronitrobenzene and the p-chloronitrobenzene are respectively monitored, and the results are shown in a graph 13 and a graph 14. As shown in fig. 13, in the system added with gallic acid, ascorbic acid, protocatechuic acid, oxalic acid, or mixed solution of tartaric acid and hydrogen peroxide, the reaction time was 72 hours, and the degradation rates of o-chloronitrobenzene in the soil were 41%, 93%, 55%, 78% and 64%, respectively. As shown in fig. 14, in the system added with gallic acid, ascorbic acid, protocatechuic acid, oxalic acid, or a mixed solution of tartaric acid and hydrogen peroxide, the degradation rates of p-chloronitrobenzene in the soil were 47%, 90%, 61%, 89% and 70%, respectively, after 48 hours of reaction.
Claims (6)
1. An in-situ chemical oxidation remediation method for organic contaminated site soil based on iron cycle regulation and control is characterized by comprising the following steps: adding a mixed solution of natural organic micromolecules and hydrogen peroxide into the soil of the organic contaminated site to be repaired, and performing in-situ chemical oxidation repair on the soil of the organic contaminated site by using naturally-occurring iron minerals in the natural organic micromolecules activated soil as effective iron sources for decomposing the hydrogen peroxide, wherein the concentration of the natural organic micromolecules in the mixed solution is 2-50 mmol/L; the concentration of the hydrogen peroxide in the mixed solution is 100-1000 mmol/L; the natural organic small molecular substance is selected from one of gallic acid, ascorbic acid, protocatechuic acid and a mixture thereof.
2. The method of claim 1, wherein: the adding amount of the mixed solution of the natural organic micromolecules and the hydrogen peroxide is 0.4-10mL/g of organic contaminated site soil.
3. The method of claim 1, wherein: after the organic contaminated site soil is sampled, a uniform soil sample is formed after freeze-drying, smashing and grinding.
4. The method of claim 1, wherein: the organic contaminants include, but are not limited to, o-chloronitrobenzene, p-chloronitrobenzene.
5. The method of claim 1, wherein: the organic contaminated site soil is repaired after the mixed solution of the natural organic micromolecules and the hydrogen peroxide is added, and the system is not stirred.
6. The method of claim 1, wherein: the mixed solution of natural organic micromolecules and hydrogen peroxide is added into soil for remediation, and the pH value in a system does not need to be adjusted.
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| CN107381766A (en) * | 2017-07-31 | 2017-11-24 | 华中师范大学 | A kind of method that natural organic molecule promotes persulfate activation repairing organic material contaminated soil and underground water |
| CN107935355A (en) * | 2017-11-24 | 2018-04-20 | 华中师范大学 | A kind of method for promoting municipal sludge deep dehydration based on ferrikinetics |
| CN108380661A (en) * | 2018-01-30 | 2018-08-10 | 华中师范大学 | A kind of method of persulfate and hydrogen peroxide compound system showering organic pollution soil |
| CN108405600A (en) * | 2018-04-23 | 2018-08-17 | 华中师范大学 | A kind of method of sodium peroxydisulfate and hydrogen peroxide compound system in-situ immobilization organic pollution soil |
| CN110773559B (en) * | 2019-11-08 | 2022-04-01 | 华中师范大学 | Method for restoring organic pollutant soil in ectopic mode through micromolecule acid coupling reduction-oxidation integration |
| CN111451266A (en) * | 2020-03-14 | 2020-07-28 | 华中师范大学 | Site water and soil cooperative remediation method and device based on iron circulation regulation |
| CN111426738B (en) * | 2020-03-14 | 2022-12-02 | 华中师范大学 | Electrochemical in-situ monitoring device and method for soil/underground water remediation process |
| CN111451267B (en) * | 2020-03-14 | 2022-06-17 | 华中师范大学 | Electrochemical in-situ automatic control contaminated site remediation system and method |
| CN115069758A (en) * | 2022-06-17 | 2022-09-20 | 温州大学 | Method for extracting cadmium in polluted soil by using gallic acid organic solution |
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| CN104511476A (en) * | 2013-10-08 | 2015-04-15 | 南京农业大学 | Method for increasing speed of oxidative degradation of organic pollutant in soil |
| CN105710125A (en) * | 2016-04-21 | 2016-06-29 | 济南大学 | Chemical repairing method for organic pollution soil |
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| CN104511476A (en) * | 2013-10-08 | 2015-04-15 | 南京农业大学 | Method for increasing speed of oxidative degradation of organic pollutant in soil |
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| CN105834207A (en) * | 2016-05-20 | 2016-08-10 | 上海化工研究院 | Method for combined remediation of organic matter polluted soil |
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