CN113522955A - In-situ remediation method for soil polluted by volatile organic compounds - Google Patents
In-situ remediation method for soil polluted by volatile organic compounds Download PDFInfo
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Abstract
The invention provides an in-situ remediation method for soil polluted by volatile organic compounds, which comprises the steps of taking persulfate as an oxidant, mixing an organic solvent and an alkaline solution to obtain a compound agent, injecting a mixture of persulfate and the compound agent in a certain proportion into the soil polluted by the organic compounds, uniformly stirring, and carrying out in-situ oxidative degradation reaction for 1-21 days in a closed manner. The use of the compound agent enables organic pollutants to be well dispersed in an organic solvent-alkaline solution to form a homogeneous system, the full contact between the oxidant and the organic pollutants is promoted, and the compound agent with a proper proportion can enhance the reaction rate of the oxidant and the volatile organic pollutants in the reaction system, so that the compound agent has an obvious degradation effect on various organic matters, and the organic pollutants are efficiently degraded.
Description
Technical Field
The invention relates to the technical field of organic matter contaminated soil remediation, in particular to an in-situ remediation method for volatile organic matter contaminated soil.
Background
Soil is a multi-medium complex system consisting of solid-liquid-gas-organisms and is one of the most important natural resources on which human beings live. In recent years, organic pollutants, such as Volatile Organic Compounds (VOCs) and semi-volatile organic compounds (SVOCs), directly or indirectly enter the soil environment due to combustion of fossil fuels, leakage of petroleum, stacking of agricultural and industrial solid wastes of industrial sewage and sludge, and widespread use of pesticides. The VOCs are precursor materials of photochemical smog and comprise benzene, toluene, ethylbenzene, dimethylbenzene, 1,3, 5-trimethylbenzene, 1,2, 4-trimethylbenzene, chlorobenzene, 1,2, 4-trichlorobenzene, chloroform and the like. SVOCs mainly include naphthalene, 1, 4-dichlorobenzene, benzo [ a ] pyrene, hexachlorobenzene, 2-methylnaphthalene, benzo (b) fluoranthene, dibenzo (a, h) anthracene, etc., and because of their benzene ring structure, the toxicity increases with the increase of the benzene ring, and they are extremely stable in the environment and difficult to degrade, and they mainly appear in areas such as coke-oven plants, pesticide plants, chemical plants, etc. The organic pollutants have higher carcinogenic, teratogenic and mutagenic effects, can not only reduce the yield of crops and even kill the crops when being left in soil, but also can enter a food chain through plants or animals, thereby bringing serious influence on the survival and health of the human beings.
Summarizing the treatment or restoration method related to soil organic pollution in recent decades at home and abroad, the method can be divided into two modes of in-situ restoration and ex-situ restoration according to restoration places. Compared with ex-situ remediation, the in-situ remediation can be used for remedying deep soil, the contaminated soil is directly remediated or treated at the site where the contamination occurs without excavating and moving the contaminated soil, and the method has the characteristics of economy, effectiveness, small engineering quantity, convenience in operation and small influence on the surrounding environment. The soil in-situ remediation technology mainly comprises an in-situ physical remediation method, an in-situ chemical remediation method and an in-situ biological remediation method, wherein the in-situ chemical remediation method is emphasized by people due to the characteristics of short remediation period, quick response, low cost, good treatment effect and the like.
The in-situ chemical oxidation technology is a process for realizing soil purification by adding chemical agents (Fenton, ozone, hydrogen peroxide, persulfate, potassium permanganate and the like) into polluted soil to enable the chemical agents to perform chemical oxidation reaction with pollutants to generate micromolecular substances with lower toxicity or easy degradation. Compared with the traditional oxidant, the persulfate advanced oxidation technology has the characteristics of good stability, high safety, wide pH value application range, slow and mild oxidation action, wide influence range, environmental friendliness and the like, the active components of the persulfate advanced oxidation technology exist in the environment for a long time, and the half-life period of the activated persulfate is 10-21 days, so that the persulfate advanced oxidation technology is beneficial to underground transportation of the persulfate advanced oxidation technology. Chinese patent (CN 106670222A) utilizes the combination of ferrous iron and hydrogen peroxide to activate persulfate so as to generate sulfate radicals and hydroxyl radicals with strong oxidizing property, thereby realizing the oxidative degradation of organochlorine pesticides in soil. The technology improves the generation amount of free radicals, reduces the quenching effect on active free radicals, and has wide pH application range and obvious oxidative degradation effect. However, in order to improve the degradation rate of pollutants in soil, a large amount of H is often required to be added2O2Increased treatment costs, and strong oxidizing agent H2O2The transportation and storage of the oil tank also have potential safety hazards.
In addition, Chinese patent (CN 111299313A) provides a sodium persulfate hydrothermal oxidation remediation method for organic contaminated soil, the method places the medicated soil in a hydrothermal reaction device, seals the hydrothermal reaction device, and heats up to 120-450 ℃ to complete soil remediation, the method greatly shortens the process flow, is convenient for engineering popularization and application, and the method is suitable for soil ex-situ remediation, the contaminated soil needs to be excavated or extracted from the original location where the site is contaminated, and is transported or transferred to other places for treatment and remediation, compared with soil in-situ remediation, the method has the defects of high treatment cost, large engineering quantity, high temperature and the like.
The occurrence mode of organic matters in soil determines that the organic matters in the soil are more difficult to remove than to treat in water phase and liquid phase, the adsorption-desorption process of the organic matters by the soil directly influences the degradation of the organic matters, and the desorption process is more difficult to carry out than the adsorption process. In the process of advanced oxidative degradation of organic pollutants, as most of the organic pollutants have smaller polarity or belong to nonpolar substances, the organic pollutants and water form two phases, so that the active components cannot be in full contact with the organic pollutants, and the organic pollutants in soil cannot be effectively degraded. Particularly, the addition of a large amount of inorganic salt oxidant not only hardly improves the remediation effect, but also causes economic cost increase and secondary soil pollution.
Disclosure of Invention
The invention aims to provide an in-situ remediation method for soil polluted by volatile organic compounds, which can promote full contact between an oxidant and organic pollutants, so as to enhance the reaction rate of the oxidant and the volatile organic pollutants in a reaction system and realize efficient degradation of the organic pollutants.
Based on the problems, the technical scheme provided by the invention is an in-situ remediation method for soil polluted by volatile organic compounds, persulfate is used as an oxidant in raw materials, an organic solvent and an alkaline solution are mixed to be used as a compound agent, under the normal temperature condition, the oxidation effect of persulfate on the organic compounds is not obvious, the oxidation of active oxygen species generated after the persulfate is activated is higher than that of the traditional Fenton reagent, and sulfate radicals SO are generated4 ·-The oxidation-reduction potential of the organic acid is 2.5-3.1V, and the organic acid reacts with the organic matters more thoroughly. The persulfate can be activated to generate a multi-free radical system, and the specific process is as follows:
S2O8 2-in a strong alkaline environment, hydrolysis generates hydroperoxyl ions HO2 -And SO4 2-See the following formula (1):
HO2 -and further with S2O8 2-Oxidation reduction reaction to generate SO4 ·-、SO4 2-And O2 ·-See the following formula (2):
in a strongly alkaline environment, SO4 ·-May also be combined with OH-Reacting, and when the pH value is more than 8.5, SO4 ·-Conversion to. OH, see formula (3):
persulfate can be decomposed into sulfate radical SO4 ·-Then further converted into hydroxyl radical OH to compensate SO4 ·-The lack of selectivity makes it have obvious degradation effect on various organic matters and great potential in the field of soil pollution.
The organic solvent is used as an auxiliary reagent, can promote the desorption of the organic pollutants adsorbed on the soil, and has obvious solubilization effect on the organic pollutants. By exploring the phase diagram of the organic-organic solvent-water ternary system, a certain range of the proportion of the organic solvent to the alkaline solution can be obtained, as shown in fig. 1, an organic (toluene) -solvent (acetonitrile) -water homogeneous phase region is arranged above a solubility curve, and a two-phase region is arranged below the solubility curve. The organic matter and acetonitrile-water form a uniform and stable system in the homogeneous phase region, so that the oxidant is promoted to fully contact with the organic pollutants, and a turbid liquid of an oil phase and a water phase is formed in the two-phase region, which is not beneficial to the degradation of the organic matter. The persulfate and the compound agent in proper proportion can enhance the reaction systemThe reaction rate of the medium free radicals with the organic contaminants. Meanwhile, the compound agent can be used as a free radical initiator to activate persulfate, and persulfate can be decomposed into sulfate radical SO4 ·-Then further converted into hydroxyl radical OH to compensate SO4 ·-The lack of selectivity makes it have obvious degradation effect on various organic matters and great potential in the field of soil pollution.
The repairing method comprises the following steps:
1) weighing a certain amount of alkaline oxide or hydroxide, and fully dissolving the alkaline oxide or hydroxide in water to prepare an alkaline solution;
2) mixing an organic solvent and an alkaline solution in a volume ratio of 3: 1-1: 5 to prepare a compound agent;
3) injecting a mixture of persulfate and a compound agent in a mass ratio of 1: 100-1: 10 into soil polluted by organic matters according to a water-soil mass ratio of 3: 1-1: 5, uniformly stirring, and carrying out in-situ oxidative degradation reaction for 1-21 days in a closed manner.
Wherein the organic solvent is one or more of acetone, acetonitrile, tween 80, dimethyl sulfoxide, N-dimethylformamide and the like.
Preferably, the organic solvent is acetonitrile, and the acetonitrile has excellent solvent performance and good solubility for various organic matters. The toxicity of the compound belongs to medium toxicity, and a small amount of acetonitrile has small secondary pollution to soil and can be metabolized by nitrogen-fixing microorganisms or plants. Therefore, the acetonitrile is properly added into the persulfate solution, so that the oxidant can be promoted to be fully contacted with the organic pollutants, and the organic pollutants can be efficiently degraded.
Wherein the pH value of the compound agent is 8-14, and preferably, the pH value of the compound agent is 11-12.
Wherein the persulfate oxidant is one or more of sodium persulfate, potassium persulfate, ammonium persulfate and the like.
Wherein the concentration of the persulfate is 20-1200 mmol/L.
The invention has the advantages and beneficial effects that:
the invention has the advantages that the composition is preparedThe compounding agent can well disperse organic pollutants in an organic solvent-alkaline solution to form a homogeneous system, promote the oxidant to fully contact with the organic pollutants, and the proper proportion of the compounding agent can enhance the reaction rate of the oxidant and the volatile organic pollutants in the reaction system. Meanwhile, the compound agent can be used as a free radical initiator to activate persulfate, and persulfate can be decomposed into SO4 ·-Then further converted into OH to compensate SO4 ·-The selectivity is not enough, so that the organic pollutant degrading agent has an obvious degrading effect on various organic matters, and the organic pollutants are efficiently degraded.
The organic solvent selected by the method has small secondary pollution to soil, can be metabolized by nitrogen-fixing microorganisms or plants, and is harmless to human body and environment. The technology has the advantages of simple process, environmental protection, low cost and wide practical application prospect.
Drawings
FIG. 1 is a toluene-acetonitrile-water ternary phase diagram.
Detailed Description
The following examples are provided to illustrate specific embodiments of the present invention.
The following examples are presented to enable those skilled in the art to more fully understand the present invention and are not intended to limit the invention in any way. Because soil has a certain adsorption effect on organic matters, the actually measured degradation rate of the organic matters is called as an apparent degradation rate.
The pretreatment and analysis methods of the organic matter sample are tested according to analysis methods such as national environmental protection standard HJ 741-2015-headspace-gas chromatography for determination of volatile organic matters in soil and sediments, HJ 834-2017-gas chromatography-mass spectrometry for determination of semi-volatile organic matters in soil and sediments, HJ 1023-2019-gas chromatography-mass spectrometry for determination of 47 pesticides such as organophosphorus and pyrethroid in soil and sediments, and the like; the detection method for the organic matter degradation experiment effect adopts one or more of dichloromethane, pentane, n-hexane and cyclohexane as an extracting agent, the volume ratio of the components of the extracting agent is 2: 1-1: 2, the ultrasonic time is 10-300 min, the ultrasonic temperature is 0-35 ℃, the centrifugal speed is 3000-15000 r/min, and the centrifugal time is 1-30 min.
Example 1
100g of contaminated soil with toluene concentration of 1000mg/kg are respectively taken in a screw bottle, and 5g of Na is added simultaneously2S2O8And injecting 200g of solvent into the screw bottle of the polluted soil, stirring to uniformly mix the solvent and the polluted soil for degradation, and performing GC analysis on 21 days of reaction, wherein the extracting agents adopted for sample pretreatment are dichloromethane and n-hexane (the volume ratio is 1:1), the ultrasonic time is 30min, the ultrasonic temperature is 25 ℃, the centrifugal speed is 6000r/min, and the centrifugal time is 5 min.
(1) When the volume ratio of acetonitrile to the basic solution in the mixture was 3:1 (90mL of acetonitrile, 30mL of basic solution having a pH of 11), the apparent degradation rate of toluene was 47.29%.
(2) When the volume ratio of acetonitrile to the basic solution in the mixture was 1:1 (56mL of acetonitrile, 56mL of basic solution having a pH of 11), the apparent degradation rate of toluene was 71.62%.
(3) When the volume ratio of acetonitrile to the basic solution in the mixture was 1:1.5 (44mL of acetonitrile, 66mL of basic solution having a pH of 11), the apparent degradation rate of toluene was 99.39%.
(4) When the volume ratio of acetonitrile to the basic solution in the mixture was 1:5 (44mL of acetonitrile, 66mL of basic solution having a pH of 11), the apparent degradation rate of toluene was 35.22%.
(5) When no combination formulation was used (50g solvent in 50mL deionized water), the apparent degradation rate of toluene was only 21.69%.
This example compares the effect of different formulation ratios and no formulation on the degradation of toluene in soil. The result shows that the oxidative degradation effect of the compound agent used as a free radical initiator on the toluene in the soil is obviously better than that of a reaction system without the compound agent, and the degradation effect of the toluene is the highest (99.39%) when the volume ratio of acetonitrile to an alkaline solution in the compound agent is 1: 1.5.
Example 2
Respectively taking 100g of the polluted soil with the ethylbenzene concentration of 1000mg/kg in a screw-top bottle, and simultaneously taking 5g of Na2S2O8And 100g of solvent is injected into the screw bottle for the polluted soilStirring to mix the mixture evenly for degradation, and carrying out GC analysis on the 21 st day of reaction, wherein the extracting agents adopted for sample pretreatment are dichloromethane and pentane (the volume ratio is 1:1), the ultrasonic time is 20min, the ultrasonic temperature is 20 ℃, the centrifugal speed is 8000r/min, and the centrifugal time is 10 min.
(1) When acetonitrile is used as an auxiliary solvent, and the volume ratio of the acetonitrile to the alkaline solution in the compound agent is 1:1.5 (44mL of acetonitrile to 66mL of alkaline solution with the pH value of 12), the apparent degradation rate of the ethylbenzene is 93.86%.
(2) When the volume ratio of acetone to alkaline solution in the compound agent is 1:1.5 (44mL of acetone to 66mL of alkaline solution with pH of 12), the apparent degradation rate of ethylbenzene is 43.61%.
(3) When the volume ratio of tween 80 to the alkaline solution in the compound agent is 1:1.5 (39mL of tween 80 and 58mL of alkaline solution with the pH value of 12) with tween 80 as an auxiliary solvent, the apparent degradation rate of the ethylbenzene is 61.96%.
(4) When dimethylsulfoxide was used as an auxiliary solvent and the volume ratio of dimethylsulfoxide to an alkaline solution in the compounded agent was 1:1.5 (38mL of a solution of dimethylsulfoxide and 58mL of an alkaline solution having a pH of 12), the apparent degradation rate of ethylbenzene was 47.11%.
(5) When N, N-dimethylformamide was used as an auxiliary solvent and the volume ratio of N, N-dimethylformamide to the alkaline solution in the mixture was 1:1.5 (40mL of N, N-dimethylformamide to 62mL of alkaline solution having a pH of 12), the apparent degradation rate of ethylbenzene was 56.66%.
This example compares the effect of different auxiliary solvents on the degradation of ethylbenzene in soil. The result shows that the oxidative degradation effect is obviously better than that of other organic solvents when the acetonitrile is used as the auxiliary solvent.
Example 3
Respectively placing 100g of contaminated soil with p-xylene concentration of 1000mg/kg in a screw bottle, mixing acetonitrile and alkaline solution (pH 11) at a volume ratio of 1:1.5 to obtain a mixture, and adding a certain amount of Na2S2O8And 100g of the compound agent is injected into the screw bottle of the polluted soil, the mixture is stirred to be uniformly mixed for degradation, GC analysis is carried out on the 21 st day of reaction, wherein the extracting agent adopted for sample pretreatment is dichloroMethane and n-hexane (volume ratio of 1:1), ultrasonic treatment time of 30min, ultrasonic treatment temperature of 25 deg.C, centrifugal rotation speed of 6000r/min, and centrifugal treatment time of 5 min.
(1)Na2S2O8When the amount of the catalyst added was 3g, the apparent degradation rate of p-xylene was 64.75%.
(2)Na2S2O8When the amount of the catalyst added was 5g, the apparent degradation rate of p-xylene was 95.37%.
(3)Na2S2O8When the amount of the catalyst added was 8g, the apparent degradation rate of p-xylene was 38.39%.
(4)Na2S2O8When the amount of the catalyst added was 10g, the apparent degradation rate of p-xylene was 24.51%.
This example compares the effect of persulfate concentration on the degradation effect of para-xylene in soil. The results show that the apparent degradation rate of p-xylene in soil increases with increasing persulfate concentration within a certain range, and that once this range is exceeded, the apparent degradation rate of p-xylene in soil decreases with increasing persulfate concentration.
Example 4
Respectively placing 100g of contaminated soil with naphthalene concentration of 1000mg/kg in screw-top bottle, mixing acetonitrile and alkaline solution (pH 11) at volume ratio of 1:1.5 to obtain mixture, and adding 5g of Na2S2O8And 50g of the compound agent is injected into the screw bottle of the polluted soil, the mixture is stirred to be uniformly mixed for degradation, GC analysis is carried out on 21 days of reaction, wherein an extracting agent adopted for sample pretreatment is dichloromethane and n-hexane (the volume ratio is 1:1), the ultrasonic time is 30min, the ultrasonic temperature is 20 ℃, the centrifugal speed is 6000r/min, and the centrifugal time is 5 min.
(1) When the pH value of the compound agent is 8, the apparent degradation rate of naphthalene is 53.75.
(2) When the pH of the compound agent is 11, the apparent degradation rate of naphthalene is 81.25%.
(3) When the pH of the compound agent is 12, the apparent degradation rate of naphthalene is 96.42%.
(4) When the pH value of the compound agent is 14, the apparent degradation rate of naphthalene is 42.76%.
This example compares the effect of the pH of the combination on the degradation of naphthalene in soil. The result shows that the increase of the pH value of the compound agent is beneficial to the improvement of the apparent degradation rate of the naphthalene in the soil, and when the pH alkalinity of the compound agent is excessively increased, the apparent degradation rate of the naphthalene in the soil is reduced.
Example 5
100g of contaminated soil with a concentration of 1000mg/kg of 1, 4-dichlorobenzene was taken in each case, acetonitrile and an alkaline solution (pH 11) were mixed in a volume ratio of 1:1.5 as a mixture, and 20g of Na was added simultaneously2S2O8And 200g of the compound agent are injected into the screw bottle of the polluted soil, the mixture is stirred to be uniformly mixed for degradation, GC analysis is carried out after reaction for a period of time, wherein the extracting agent adopted for sample pretreatment is dichloromethane and cyclohexane (the volume ratio is 1:1), the ultrasonic time is 30min, the ultrasonic temperature is 20 ℃, the centrifugal speed is 6000r/min, and the centrifugal time is 5 min.
(1) On the 3 rd day of the reaction, the apparent degradation rate of 1, 4-dichlorobenzene reached 43.79%.
(2) At the 10 th day of the reaction, the apparent degradation rate of 1, 4-dichlorobenzene reached 67.31%.
(3) On the 21 st day of the reaction, the apparent degradation rate of 1, 4-dichlorobenzene reached 88.25%.
This example compares the effect of reaction time on the degradation of 1, 4-dichlorobenzene in soil. The results show that the apparent degradation rate of 1, 4-dichlorobenzene increases with the increase of the reaction time.
Although the embodiments of the present invention have been described in detail, the description is only for the preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (6)
1. An in-situ remediation method for soil polluted by volatile organic compounds, which uses persulfate as an oxidant in raw materials and is characterized in that: mixing an organic solvent and an alkaline solution to obtain a compound agent, wherein the repairing method comprises the following steps:
1) weighing a certain amount of alkaline oxide or hydroxide, and fully dissolving the alkaline oxide or hydroxide in water to prepare an alkaline solution;
2) mixing an organic solvent and an alkaline solution in a volume ratio of 3: 1-1: 5 to prepare a compound agent;
3) injecting a mixture of persulfate and a compound agent in a mass ratio of 1: 100-1: 10 into the soil polluted by organic matters in a water-soil mass ratio of 3: 1-1: 5, uniformly stirring, and carrying out in-situ oxidative degradation reaction for 1-21 days in a closed manner.
2. The in-situ remediation method of volatile organic compound-contaminated soil according to claim 1, wherein: the organic solvent is one or more of acetone, acetonitrile, tween 80, dimethyl sulfoxide, N-dimethylformamide and the like.
3. The in-situ remediation method of volatile organic compound-contaminated soil according to claim 2, wherein: the organic solvent is acetonitrile.
4. The in-situ remediation method of volatile organic compound-contaminated soil according to claim 1, wherein: the pH value of the prepared compound agent is 8-14.
5. The in-situ remediation method of volatile organic compound-contaminated soil according to claim 1, wherein: the persulfate oxidizer is one or more of sodium persulfate, potassium persulfate, ammonium persulfate and the like.
6. The in-situ remediation method of volatile organic compound-contaminated soil according to claim 5, wherein: the concentration of the persulfate is 20-1200 mmol/L.
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| CN117884463A (en) * | 2024-01-18 | 2024-04-16 | 上海久澄环境工程有限公司 | Treatment of diethyl sulfide and diethyl disulfide in soil by normal temperature desorption method |
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