CN110773559A - Method for restoring organic pollutant soil in ectopic mode through micromolecule acid coupling reduction-oxidation integration - Google Patents
Method for restoring organic pollutant soil in ectopic mode through micromolecule acid coupling reduction-oxidation integration Download PDFInfo
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Abstract
The invention belongs to the field of environmental chemistry, and particularly relates to a method for restoring organic pollutant soil in an ectopic mode through micromolecule acid coupled reduction-oxidation integration. In the first stage, zero-valent iron material and natural organic small molecular acid are added into the soil which is piled up in a centralized way, stirred and mixed evenly, and reduction reaction is carried out for a period of time, wherein the stage is mainly used for reducing target pollutants; and in the second stage, adding hydrogen peroxide or a mixed solution of the hydrogen peroxide and the small molecular acid, stirring and mixing uniformly, and carrying out Fenton oxidation removal on the reduced organic pollutant soil. The natural organic small molecular acid coupling agent added in the method plays a role in coupling two stages of reduction reaction and oxidation reaction, can simultaneously enhance the reduction and oxidation efficiency, finally realizes the reduction-oxidation integrated efficient removal of organic pollutants, solves the problem of low removal efficiency by singly utilizing the reduction or oxidation technology, and has better organic matter polluted soil remediation effect.
Description
Technical Field
The invention belongs to the field of environmental chemistry, and particularly relates to a reduction-oxidation integrated ex-situ remediation method for organic pollutant soil by using natural organic small molecular acid as a coupling agent to simultaneously enhance reduction and oxidation efficiencies, which is suitable for remediation of organic pollutant contaminated soil in industries such as industry, agriculture, medicine and the like.
Background
With the rapid development of industrialization and urbanization, the problem of soil pollution in China is becoming more and more serious, wherein, because the problem of organic pollution caused by the industries such as pesticide, coal chemical industry, petrochemical industry and the like is very serious, the remediation of the soil pollution caused by organic pollution becomes an unbearable big thing. Therefore, the development of effective organic soil remediation technology has been the focus of research in the field of environmental remediation.
Among the technologies for treating soil organic pollutants by using chemical methods, reduction and oxidation are two most basic approaches, and are suitable for treating various organic pollutants with high and low concentrations. However, single reduction or oxidation techniques have some disadvantages for the removal of some specific contaminants. For example, for the degradation of some chlorinated hydrocarbon or nitroaromatic pollutants, a single reduction technology is adopted to control the concentration of a target pollutant, but some reduction products with stronger toxicity are generated, so that more serious environmental pollution is caused, and more importantly, the single reduction technology cannot achieve the mineralization of organic pollutants basically; and by adopting a single oxidation technology, such as directly adding hydrogen peroxide, persulfate and the like, the pollutants are difficult to effectively remove or mineralize, and the aim of repairing is difficult to achieve. Taking chloronitrobenzene as an example, it is widely used in the national defense, printing and dyeing, plastics, pesticides and pharmaceutical industries, and the annual production of nitrochlorobenzene in china accounts for 60% of the total global production, but it has strong carcinogenicity and mutagenicity, and poor biodegradability, seriously threatens the safety of ecological environment, and this kind of compound has been listed as one of the priority control pollutants by the united states Environmental Protection Agency (EPA). Studies have shown that the nitro group (-NO) of chloronitrobenzene
2) Has stronger electron-withdrawing property and is a passivation group, so that the chloronitrobenzene has stable chemical structure and is difficult to be oxidized, degraded and mineralized. Although the single reduction technology can effectively carry out nitro reduction and even dechlorination of chloronitrobenzene, the single reduction technology is easy to generate chloroaniline and other intermediate products with strong toxicity, and cannot achieve effective and thorough repair. Against the prior artIn addition, the method for restoring the organic pollutant soil in a reduction-oxidation integrated ectopic mode by using natural organic micromolecule acid as a coupling agent to enhance the reduction and oxidation efficiencies simultaneously is provided, namely under the condition of adding the natural micromolecule acid, firstly reducing the compounds to obtain a reduction intermediate product, and then further oxidizing the intermediate product with stronger reducibility and the target pollutant which is not completely reacted by using an oxidation reaction, so that the target pollutant can be effectively removed and mineralized.
Disclosure of Invention
The invention provides a method for restoring organic pollutant soil in a reduction-oxidation integrated ectopic mode through coupling of small molecular acid, aiming at the defects of the prior art.
According to the reduction-oxidation integrated method with the natural organic small molecular acid as the coupling agent, the small molecular acid in the reduction stage can be used for enhancing the electron transfer rate and the electron selectivity of zero-valent iron in the reduction stage, the small molecular acid in the oxidation stage can be used as an activating agent for achieving the efficient circulation of Fe (III)/Fe (II) in the oxidation stage, the reduction efficiency and the oxidation efficiency can be enhanced simultaneously, and the purpose of efficiently chemically repairing the polluted soil can be achieved more effectively through the reduction-oxidation integrated technology.
The technical scheme adopted by the invention for solving the problems is as follows:
a method for restoring organic pollutant soil in different positions by micromolecule acid coupled reduction-oxidation integration includes adding zero-valent iron materials and natural organic micromolecule acid into soil which is piled up in a concentrated mode, stirring and mixing uniformly, carrying out reduction reaction for a period of time, adding hydrogen peroxide or mixed solution of hydrogen peroxide and natural organic micromolecule acid, stirring and mixing uniformly, and carrying out Fenton oxidation removal on the reduced organic pollutant soil.
According to the scheme, the natural organic small molecular acid is one or a mixture of more than one of ascorbic acid, oxalic acid, citric acid and protocatechuic acid.
According to the scheme, the same natural organic micromolecular acid can be added in the reduction stage and the oxidation stage, and two different micromolecular acids can also be added.
According to the scheme, the adding amount of the natural organic small molecular acid is 0.2-2 wt% of the soil to be repaired in the reduction stage, and the adding amount of the natural organic small molecular acid is 0-2 wt% of the soil to be repaired in the oxidation stage.
According to the scheme, the reaction time after the zero-valent iron material and the natural organic micromolecular acid are added is 0-7 days; adding hydrogen peroxide or the mixed solution of hydrogen peroxide and natural organic small molecular acid for 3-14 days.
According to the scheme, the zero-valent iron material is commercial iron powder, or one of zero-valent iron powder pretreated by boric acid, phosphoric acid, oxalic acid, sulfur powder or biochar and a mixture thereof, and the pretreatment is to perform surface modification or load treatment on the commercial iron powder in a mode of dipping or ball milling by boric acid, phosphoric acid, oxalic acid, sulfur powder or biochar solution and the like.
According to the scheme, the adding amount of the zero-valent iron material is 0.2-5 wt% of the amount of the soil to be repaired.
According to the scheme, the adding quality of the hydrogen peroxide is 0.6-3.6 wt% of the soil to be repaired according to the content of the effective hydrogen peroxide.
According to the scheme, the mass percentage concentration of the hydrogen peroxide in the mixed solution of the hydrogen peroxide and the natural small molecular acid is 3.0-18% (diluted by water to the required concentration) according to the content of the effective hydrogen peroxide, and the mass percentage concentration of the natural organic small molecular acid in the mixed solution is 1-10%.
According to the scheme, the organic pollutants comprise but are not limited to chloronitrobenzene and chlorobenzene series.
According to the scheme, the soil is timely stirred in the reduction and oxidation removal stages of the organic pollutants.
The technical principle of the invention is as follows:
the method carries out ex-situ remediation on the organic pollutant soil by using a reduction-oxidation integrated technology which takes natural organic micromolecule acid as a coupling agent and simultaneously enhances the reduction and oxidation efficiencies. Specifically, firstly, adding a zero-valent iron material and natural organic small molecular acid into the soil which is piled up in a centralized way, stirring and mixing uniformly, and mainly reducing target pollutants in the stage; then hydrogen peroxide or a mixed solution of hydrogen peroxide and a small molecular acid is injected into the organic pollutant soil, the organic pollutant soil after reduction is subjected to oxidation treatment, the organic pollutant soil is stirred and mixed uniformly and then reacts for 1 to 2 weeks, and the treated soil is stirred in time. According to the invention, firstly, the micromolecular acid is added in the reduction stage, the inherent reducibility, electron-rich characteristics and the like of the micromolecular acid are utilized, the electron transfer rate and electron selectivity of zero-valent iron in the reduction stage are enhanced through the regulation and control effect of the micromolecular acid, and the high-efficiency reduction of the zero-valent iron material pollutants is realized, so that the zero-valent iron materials are converted into reduction products which are easier to oxidize; meanwhile, the small molecular acid in the oxidation stage can be used as an activator and simultaneously realize the high-efficiency circulation of Fe (III)/Fe (II) in the Fenton oxidation stage, so that hydrogen peroxide is more efficiently decomposed to generate OH, and finally, the target pollutant and the reduction product which are not completely reacted are continuously subjected to high-efficiency oxidation reaction, and the high-efficiency mineralization of the organic pollutant is realized.
The invention has the advantages that:
(1) according to the method, the reduction-oxidation coupling technology is adopted to carry out ex-situ remediation on the organic matter contaminated soil, the natural organic micromolecule acid is added at the same time, the reduction efficiency and the oxidation efficiency can be simultaneously enhanced by adding the natural organic micromolecule acid, the effect of coupling two stages of reduction reaction and oxidation reaction is achieved, the reduction-oxidation integrated efficient removal of the organic pollutants is finally realized, the problem of low removal efficiency due to the single utilization of the reduction or oxidation technology is solved, and the remediation effect of the organic matter contaminated soil is good.
(2) The method has the advantages of good repairing effect, simple process, cost saving and no secondary pollution.
(3) The invention uses the iron powder pretreated by the methods of boric acid, phosphoric acid, oxalic acid, sulfur powder, biochar and the like to enhance the capability of the iron powder in reducing organic matters and promote the activation of H
2O
2Ability to generate OH. The modification not only improves the reduction efficiency in the reduction stage, but also promotes the efficient oxidative degradation mineralization in the oxidation stage.
Drawings
FIG. 1 is a diagram showing the effect of ex-situ remediation of chloronitrobenzene contaminated soil by the method of the present invention;
FIG. 2 is a diagram showing the effect of ex-situ remediation of chlorobenzene-contaminated soil by using boronized zero-valent iron.
Detailed Description
The present invention will be described in detail with reference to specific examples, which are provided for illustration only and are not intended to limit the scope of the present invention.
Example 1 reduction, oxidation and reduction-oxidation coupled technology ectopically remediation of chloronitrobenzene contaminated soil
The chloronitrobenzene contaminated soil is taken from a pharmaceutical and chemical engineering contaminated site in Wuhan, and after sampling, the contaminated soil is air-dried, crushed and sieved to form a uniform soil sample. Aiming at restoring the soil of the chloronitrobenzene polluted site, adding 2 wt% of iron powder into 300g of soil, stirring and mixing uniformly, and then adding an ascorbic acid aqueous solution with the mass concentration of 7.5% (the mass of the ascorbic acid is 0.5 wt% of the soil); after reacting for three days, adding hydrogen peroxide solution with effective mass concentration of 13.5% (the effective hydrogen peroxide mass is 1.8 wt% of the soil), stirring and mixing uniformly, and continuing to react for one week (recorded as reduction oxidation 1). Control experiments were also set up as follows: (1) adding iron powder as a reducing agent, and reacting for one week without adding ascorbic acid (marked as reduction 1); (2) adding iron powder as a reducing agent, and adding ascorbic acid to react for one week (marked as reduction 2); (3) adding iron powder as a reducing agent in a reduction stage, adding hydrogen peroxide in an oxidation stage after reducing for three days without adding ascorbic acid, and continuously reacting for one week (marked as reduction oxidation 2); (4) and (4) directly adding hydrogen peroxide without a reduction stage, and carrying out oxidation reaction for one week (marked as oxidation 1). As shown in figure 1, after one week of reaction, the removal rates of chloronitrobenzene after the reduction 1 and the reduction 2 treatment are respectively 40% and 52%; the efficiency of reducing and oxidizing 1 and reducing and oxidizing 2 to remove chloronitrobenzene is 89 percent and 70 percent; and the removal rate of chloronitrobenzene after only one week of treatment with oxidation 1 without reduction stage was 36%.
Example 2 reduction, oxidation and reduction-oxidation coupled technology ectopically remediation of chlorobenzene contaminated soil
The chlorobenzene polluted soil is taken from a pesticide chemical polluted site in Wuhan province, and mainly contains chlorobenzene, 1, 4-dichlorobenzene and 1, 2-dichlorobenzene. After sampling, the polluted soil is air-dried, crushed and sieved to form a uniform soil sample. Aiming at the restoration of the soil of the organochlorine pesticide polluted site, adding 3.3 wt% of iron boride powder (obtained by ball milling of boric acid and iron powder) and a protocatechuic acid aqueous solution with the mass concentration of 4% (the mass of protocatechuic acid is 0.2 wt% of the soil) into 300g of soil, and uniformly stirring and mixing; after reacting for three days, adding a mixed aqueous solution of hydrogen peroxide and protocatechuic acid, wherein the effective mass concentration of the hydrogen peroxide in the solution is 16 percent, and the mass concentration of the protocatechuic acid is 3 percent (the mass of the effective hydrogen peroxide is 1.2 percent of the mass of the soil, and the mass of the protocatechuic acid is 0.3 percent of the mass of the soil), stirring and mixing uniformly, and starting the reaction in the oxidation stage (marked as reduction and oxidation 1).
Control experiments were also set up as follows: (1) adding iron boride powder as a reducing agent, and reacting for one week without adding protocatechuic acid (marked as reduction 1); (2) adding iron boride powder as a reducing agent, adding protocatechuic acid, and reacting for one week (marked as reduction 2); (3) adding iron boride powder as a reducing agent in a reduction stage, adding hydrogen peroxide in an oxidation stage after reducing for three days without adding protocatechuic acid, and continuing to react for one week (marked as reduction oxidation 2); (4) adding iron boride powder as a reducing agent in a reduction stage, adding protocatechuic acid for reduction for three days, only adding hydrogen peroxide in an oxidation stage, and continuously reacting for one week (marked as reduction oxidation 3); (5) adding iron boride powder as a reducing agent in a reduction stage, adding protocatechuic acid, reducing for three days, adding hydrogen peroxide in an oxidation stage, and adding protocatechuic acid to continue to react for one week (marked as reduction oxidation 4); (6) in the non-reduction stage, hydrogen peroxide is directly added for oxidation reaction for one week (marked as oxidation 1); (7) without the reduction stage, hydrogen peroxide and protocatechuic acid were added for oxidation for one week (noted as oxidation 2). As shown in fig. 2, after one week of reaction, the chlorobenzene removal rates after reduction 1 and reduction 2 treatment were 42% and 56%, respectively; the removal rate of p-chlorobenzene by redox 1, redox 2, redox 3 and redox 4 is 88%, 68%, 80% and 70%; and the removal rate of chlorobenzene after one week of treatment by oxidation 1 and oxidation 2 is 39% and 50% respectively, except for the reduction stage.
Claims (10)
1. A method for restoring organic pollutant soil in a reduction-oxidation integrated ectopic mode through coupling of micromolecule acid is characterized in that: adding a zero-valent iron material and natural organic micromolecular acid into the soil which is piled up intensively, stirring and mixing uniformly, carrying out reduction reaction for a period of time, then adding hydrogen peroxide or a mixed solution of the hydrogen peroxide and the natural organic micromolecular acid, stirring and mixing uniformly, and carrying out Fenton oxidation removal on the reduced organic pollutant soil.
2. The method of claim 1, wherein: the natural organic small molecular acid is one or a mixture of more than one of ascorbic acid, oxalic acid, citric acid and protocatechuic acid.
3. The method according to claim 1 or 2, characterized in that: the same small molecule acid is added in the reduction stage and the oxidation stage, or two different small molecule acids are added.
4. A method according to claim 1 or 2 or 3, characterized in that: the adding amount of the natural organic small molecular acid is 0.2-2 wt% of the soil to be repaired in the reduction stage, and the adding amount is 0-2 wt% of the soil to be repaired in the oxidation stage.
5. The method of claim 1, wherein: the reaction time after the zero-valent iron material and the natural organic micromolecular acid are added is 0-7 days; adding hydrogen peroxide or the mixed solution of hydrogen peroxide and natural organic small molecular acid for 3-14 days.
6. The method of claim 1, wherein: the zero-valent iron material is commercial iron powder, or one of zero-valent iron powder pretreated by boric acid, phosphoric acid, oxalic acid, sulfur powder or biochar and a mixture thereof, and the pretreatment is to perform surface modification or load treatment on the commercial iron powder in a mode of dipping or ball milling by boric acid, phosphoric acid, oxalic acid, sulfur powder or biochar solution and the like.
7. The method according to claim 1 or 6, characterized in that: the dosage of the zero-valent iron material is 0.2-5 wt% of the soil to be repaired; the adding quality of the hydrogen peroxide is 0.6-3.6 wt% of the soil to be repaired according to the content of the effective hydrogen peroxide.
8. The method of claim 1, wherein: the mass percentage concentration of the hydrogen peroxide in the mixed solution of the hydrogen peroxide and the natural small molecular acid is 3.0-18% according to the content of the effective hydrogen peroxide, and the mass percentage concentration of the natural organic small molecular acid in the mixed solution is 1-10%.
9. The method of claim 1, wherein: the organic pollutants include but are not limited to chloronitrobenzene and chlorobenzene series.
10. The method of claim 1, wherein: and stirring the soil in the reduction and oxidation removal stages of the organic pollutants in time.
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| CN112320919A (en) * | 2020-10-16 | 2021-02-05 | 中国环境科学研究院 | Water body restoration method based on zero-valent iron silicide activated persulfate |
| CN112429829A (en) * | 2020-10-28 | 2021-03-02 | 暨南大学 | Reactivation stabilized layered ferric hydroxide and preparation method and application thereof |
| CN114951260A (en) * | 2022-06-22 | 2022-08-30 | 昆明理工大学 | Method for restoring organic contaminated soil by using plants rich in polyphenol |
| CN115090237A (en) * | 2022-05-18 | 2022-09-23 | 上海交通大学 | Method for converting zero-valent iron into waste plastic through photo-thermal conversion into high-value-added fuel and environment-repairing material |
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| CN112320919A (en) * | 2020-10-16 | 2021-02-05 | 中国环境科学研究院 | Water body restoration method based on zero-valent iron silicide activated persulfate |
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| CN115487831B (en) * | 2022-09-28 | 2023-11-03 | 中国科学院南京土壤研究所 | Preparation method of Fe modified material and application of Fe modified material in degradation of organic pollutants in soil by activated persulfate |
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