CN115722529A - Method for promoting Fenton reaction to repair organic contaminated soil by microwave slow-release material - Google Patents
Method for promoting Fenton reaction to repair organic contaminated soil by microwave slow-release material Download PDFInfo
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- 230000001737 promoting effect Effects 0.000 title claims abstract description 15
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- VTIIJXUACCWYHX-UHFFFAOYSA-L disodium;carboxylatooxy carbonate Chemical compound [Na+].[Na+].[O-]C(=O)OOC([O-])=O VTIIJXUACCWYHX-UHFFFAOYSA-L 0.000 claims abstract description 43
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- LMHAGAHDHRQIMB-UHFFFAOYSA-N 1,2-dichloro-1,2,3,3,4,4-hexafluorocyclobutane Chemical compound FC1(F)C(F)(F)C(F)(Cl)C1(F)Cl LMHAGAHDHRQIMB-UHFFFAOYSA-N 0.000 claims abstract description 22
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- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 19
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- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 13
- OWZIYWAUNZMLRT-UHFFFAOYSA-L iron(2+);oxalate Chemical compound [Fe+2].[O-]C(=O)C([O-])=O OWZIYWAUNZMLRT-UHFFFAOYSA-L 0.000 claims abstract description 13
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- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 36
- 238000013268 sustained release Methods 0.000 claims description 36
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- MGZTXXNFBIUONY-UHFFFAOYSA-N hydrogen peroxide;iron(2+);sulfuric acid Chemical compound [Fe+2].OO.OS(O)(=O)=O MGZTXXNFBIUONY-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a method for restoring organic contaminated soil by promoting Fenton reaction by using a microwave slow-release material, which comprises the following steps: step S1: dissolving 10 parts of sodium carboxymethylcellulose in water to prepare a 1-3% solution, adding 2-10% of bentonite, heating to 45-85 ℃ for 40-70 minutes to form a uniform viscous solution; step S2: adding 60 parts of sodium percarbonate, 6 parts of peroxide activator Tetraacetylethylenediamine (TAED), 0.5 part of stabilizer 2-hydroxyphosphonoacetic acid and 0.5 part of EDTA into the solution, quickly and uniformly stirring, filtering or centrifugally separating, drying until the quality is constant, adding 7-25 parts of ferrous sulfate or ferrous oxalate, and uniformly stirring to obtain a finished slow-release material; and finally, repairing the organic contaminated soil under an intermittent microwave condition.
Description
Technical Field
The invention relates to the field of organic contaminated soil remediation, in particular to a method for remedying organic contaminated soil by promoting Fenton reaction by using a microwave slow-release material.
Background
Soil remediation refers to the physical, chemical and biological processes of transferring, absorbing, degrading and converting pollutants in soil to reduce their concentration to an acceptable level, or converting toxic and harmful pollutants into harmless substances, and generally includes the 3 types of processes of biological remediation, physical remediation and chemical remediation.
The chemical remediation method of soil pollution is a technology of adding chemical substances into soil, and removing pollutants in the soil or reducing the biological effectiveness or toxicity of the pollutants in the soil through chemical reactions such as oxidation reduction, chelation or precipitation of heavy metals and organic matters. Mainly comprises soil solidification and stabilization, leaching, oxidation reduction and the like.
The oxidation-reduction method is widely applied to the remediation of the soil in the organic pollution site due to the rapid degradation capability of the organic pollutants. Common oxidants are ozone, hydrogen peroxide, permanganate, fenton's reagent, persulfate, and the like.
Wherein, the Fenton reagent has strong oxidizability but instability, is easy to be rapidly decomposed to generate oxygen and a large amount of heat, has very fast reaction speed with an activating agent, and can not effectively utilize the generated hydroxyl free radical (OH.); meanwhile, hydrogen peroxide is easily decomposed into oxygen and water by soil microorganisms, clay minerals, transition metal elements and the like in soil, and the oxidation is lost; in addition, the Fenton reagent is used for non-selective oxidation of soil organic matters, so that a large amount of waste of the Fenton reagent is brought, the reaction efficiency is low, and the cost is low.
In order to solve the above problems, research and consideration have been made on adopting sodium percarbonate to replace hydrogen peroxide, and regulating the rate of releasing hydrogen peroxide by regulating the decomposition rate of sodium percarbonate. For example, the method for repairing the polluted soil by using the microwave-enhanced sodium percarbonate has the advantages that the method still has an improved space due to the instability of the sodium percarbonate, the method regulates and controls the process of generating hydrogen peroxide by using the sodium percarbonate through microwaves, further generates a Fenton reaction, and simultaneously repairs the organic polluted soil, so that the oxidation efficiency is improved, the using amount of the oxidant is reduced, and the storage time of the oxidant is prolonged.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for promoting Fenton reaction to repair organic contaminated soil by using a microwave slow-release material.
The technical scheme of the invention is as follows:
a method for restoring organic contaminated soil by promoting Fenton reaction by using a microwave slow-release material comprises the following steps:
step S1: dissolving 10 parts of sodium carboxymethylcellulose in water to prepare a 1-3% solution, adding 2-10% of bentonite, and heating to 45-85 ℃ for 40-70 minutes to form a uniform and viscous solution;
step S2: adding 60 parts of sodium percarbonate, 6 parts of peroxide activator Tetraacetylethylenediamine (TAED), 0.5 part of stabilizer 2-hydroxyphosphonoacetic acid and 0.5 part of EDTA into the solution, quickly and uniformly stirring, filtering or centrifugally separating, drying until the mass is constant, adding 7-25 parts of ferrous sulfate or ferrous oxalate, and uniformly stirring to obtain a finished product of the sustained-release material;
and step S3: the sodium carboxymethylcellulose and the bentonite are in cross-linking with the sodium percarbonate to prevent the sodium percarbonate from being decomposed inefficiently due to too fast speed, so that the speed of releasing the hydrogen peroxide is slow and controllable, the sodium percarbonate and Fe (II) components in the material form a Fenton reagent, and the Fe (II) catalyzes the hydrogen peroxide to generate hydroxyl radicals, thereby realizing the degradation of pollutants;
and step S4: the stabilizer 2-hydroxyphosphonoacetic acid and EDTA are used for chelating heavy metal ions in a reaction medium and preventing the metal ions from catalyzing the decomposition reaction of sodium percarbonate;
step S5: and (5) repairing.
Preferably, the microwave in step S5 is used for promoting desorption and solubilization of soil pesticide while controlling the sodium percarbonate in the sustained-release material to release hydrogen peroxide, so as to improve the contact effect of the pollutant and the oxidant, and create favorable conditions for the oxidant to fully degrade the pollutant.
Preferably, the peroxide activator Tetraacetylethylenediamine (TAED) in step S2 is used to activate peroxide to release nascent oxygen at room temperature, thereby improving oxidation efficiency.
Preferably, in the method, the oxidant is sodium percarbonate, the catalyst is ferrous sulfate or ferrous oxalate, the cross-linking agent is sodium carboxymethylcellulose, the mineral matrix is bentonite, the peroxide activator is tetraacetylethylenediamine TAED, and the stabilizer is 2-hydroxyphosphonoacetic acid.
Preferably, said step S5 comprises the following sub-steps:
s51: putting the organic contaminated soil to be treated into a reactor, wherein the mass of the soil is 10-50 g.
S52: preparing a slow-release material aqueous solution, and stirring and mixing the slow-release material aqueous solution with the organic contaminated soil, wherein the liquid-solid ratio is 1.
S53: adjusting the pH value of the soil and water mixed environment to 3-5, and carrying out acidification treatment for 5-10 min.
S54: intermittently emitting microwaves for 5min under the condition that the microwave power is 300-850W, wherein the microwave time period and the microwave-free time period are 1.
S55: under the condition of the intermittent microwave, the microwave treatment time is 30-300 s, the standing reaction time is 0.2-1 h, and one period is formed, and the polluted soil can be repaired in a plurality of periods.
The method for promoting Fenton reaction to repair organic contaminated soil by using the microwave slow-release material has the following beneficial effects:
1. the invention combines proper proportion of cross-linking agent, activating agent, stabilizing agent and the like, and controls the slow release rate of hydrogen peroxide and Fe (II) component by combining with microwave, so as to form Fenton reagent, the slow release function prevents the sodium percarbonate component from decomposing too fast to generate hydrogen peroxide to bring about oxidant loss, and the high-efficiency slow release oxidation material with good slow release performance, high oxidant utilization rate and low cost is formed, and can be used for implementing soil remediation engineering.
2. The microwave condition simultaneously excites the sodium percarbonate component to generate hydrogen peroxide and desorbs and solubilizes the pollution component in the polluted soil to enter the soil solution, and finally the pollution component and the Fenton reagent formed by the release of the slow-release material are effectively reacted, so that the non-targeted oxidation processes of soil organic matter oxidation and the like are reduced, and the using amount of the oxidant is reduced.
3. The peroxide activator is utilized to promote the utilization rate of hydrogen peroxide, enhance the Fenton reaction efficiency, improve the oxidation efficiency and fulfill the aim of restoring the organic contaminated soil.
4. The high-efficiency slow-release oxidation material formed by the invention has good stability, prolongs the quality guarantee period of the effective components of the oxidant material, and particularly has a quality guarantee period superior to that of like products under the normal-temperature and humid conditions. The cost investment of practical application is reduced.
5. The method avoids the common problems of the classic Fenton reagent in the soil remediation process, and improves the problems of decomposition regulation and oxidation effectiveness and the like of the sodium percarbonate in the method of remedying the polluted soil by using the microwave-enhanced sodium percarbonate. The method has the advantages of high degradation efficiency, simple process conditions and no secondary pollution, and can be widely applied to the remediation of the organic contaminated soil.
Drawings
FIG. 1 is a flow chart of the method of the present invention.
FIG. 2 is a comparison of various embodiments of the present invention.
Detailed Description
The following description of the embodiments of the present invention is provided to facilitate the understanding of the present invention by those skilled in the art, but it should be understood that the present invention is not limited to the scope of the embodiments, and it will be apparent to those skilled in the art that various changes may be made without departing from the spirit and scope of the invention as defined and defined by the appended claims, and all changes that can be made by the invention using the inventive concept are intended to be protected.
As shown in FIG. 1, preparation of sustained-release Material
Oxidizing agent: sodium percarbonate
Catalyst: ferrous sulfate or ferrous oxalate
A crosslinking agent: sodium carboxymethylcellulose
Mineral matrix: bentonite clay
Peroxide activators: tetraacetylethylenediamine (TAED)
Stabilizer 2-hydroxyphosphonoacetic acid
Preparing a slow-release material:
dissolving 10 parts of sodium carboxymethylcellulose in water to prepare a 1-3% solution, adding 2-10% of bentonite, and heating to 45-85 ℃ for 40-70 minutes to form a uniform and viscous solution;
adding 60 parts of sodium percarbonate, 6 parts of peroxide activator Tetraacetylethylenediamine (TAED), 0.5 part of stabilizer 2-hydroxyphosphonoacetic acid and 0.5 part of EDTA into the solution, quickly and uniformly stirring, filtering or centrifugally separating, drying until the quality is constant, adding 7-25 parts of ferrous sulfate or ferrous oxalate, and uniformly stirring to obtain a finished product of the sustained-release material.
The organic contaminated soil remediation process comprises the following steps:
(1) Putting the organic contaminated soil to be treated into a reactor, wherein the mass of the soil is 10-50 g.
(2) Preparing a slow-release material aqueous solution, and stirring and mixing the slow-release material aqueous solution with the organic contaminated soil, wherein the liquid-solid ratio is 1.
(3) Adjusting the pH value of the soil and water mixed environment to 3-5, and carrying out acidification treatment for 5-10 min.
(4) And intermittently emitting microwaves under the condition that the microwave power is 300-850W, wherein the microwave time period and the microwave-free time period are 1.
(5) Under the condition of the intermittent microwave, the treatment time is 30-300 s, the standing reaction is 0.2-1 h to form a period, and the polluted soil can be repaired in a plurality of periods.
In the reaction system:
the microwave has the effects of controlling the sodium percarbonate in the slow-release material to release hydrogen peroxide, promoting the desorption and solubilization of soil pesticides, improving the contact effect of pollutants and an oxidant and creating favorable conditions for the oxidant to fully degrade the pollutants.
The sodium carboxymethylcellulose and the bentonite are bonded with the sodium percarbonate to prevent the sodium percarbonate from being decomposed inefficiently due to overquick speed, so that the speed of releasing the hydrogen peroxide is slow and controllable, a Fenton reagent is formed with Fe (II) components in the sodium percarbonate, and the Fe (II) catalyzes the hydrogen peroxide to generate hydroxyl radicals, thereby realizing the degradation of pollutants.
The peroxide activator Tetraacetylethylenediamine (TAED) has the functions of activating peroxide to release nascent oxygen at normal temperature and improving oxidation efficiency.
The stabilizers 2-hydroxyphosphonoacetic acid and EDTA are used to chelate the heavy metal ions in the reaction medium, preventing the metal ions from catalyzing the decomposition reaction of sodium percarbonate.
Example 1
Preparation of the sustained-release material: dissolving 1g sodium carboxymethylcellulose, adding into 33ml water for several times in small amount to obtain 3% solution, adding bentonite 2%, and heating to 85 deg.C under stirring for 40 min to obtain uniform viscous solution; and (3) when the solution is cooled to room temperature, adding 6g of sodium percarbonate, 0.6g of peroxide activator Tetraacetylethylenediamine (TAED), 0.05g of stabilizer 2-hydroxyphosphonoacetic acid and 0.05g of EDTA into the solution, quickly and uniformly stirring, freeze-drying, adding 2.5g of ferrous sulfate, grinding and uniformly stirring to obtain a finished sustained-release material 1.
And (3) repairing the toluene-polluted soil: 10g of toluene-contaminated soil to be treated having a concentration of 100mg/kg were placed in a reactor. Taking 0.5g of the slow release material finished product 1, preparing a solution, and quickly adding the solution into a reactor according to a liquid-solid ratio of 1. Adjusting the pH value of the mixed environment of the soil and the water to 3, and continuously stirring and acidizing for 5min. And (3) performing intermittent microwave treatment under the condition that the microwave power is 800W, starting the microwave for 10 seconds, pausing for 20 seconds (the ratio of the microwave time period to the microwave-free time period is 1. The operations are repeated, and the polluted soil is repaired after 1 hour.
Example 2
Preparation of the sustained-release material: dissolving 1g sodium carboxymethylcellulose, adding a small amount of sodium carboxymethylcellulose into 50ml water for multiple times to obtain 2% solution, adding bentonite 5%, and heating to 60 deg.C for 60 min under continuous stirring to obtain uniform viscous solution; and (3) when the solution is cooled to room temperature, adding 6g of sodium percarbonate, 0.6g of peroxide activator Tetraacetylethylenediamine (TAED), 0.05g of stabilizer 2-hydroxyphosphonoacetic acid and 0.05g of EDTA into the solution, quickly and uniformly stirring, freeze-drying, adding 2g of ferrous sulfate, grinding and uniformly stirring to obtain a finished sustained-release material 2.
And (3) repairing the toluene-polluted soil: 10g of toluene-contaminated soil to be treated with a concentration of 200mg/kg were placed in a reactor. Taking 1.5g of the slow release material finished product 2, preparing a solution, and quickly adding the solution into a reactor according to a liquid-solid ratio of 1. Adjusting the pH value of the mixed environment of the soil and the water to 3, and continuously stirring and acidizing for 5min. And (3) performing intermittent microwave treatment under the condition that the microwave power is 800W, starting the microwave for 10 seconds, pausing for 30 seconds (the ratio of the microwave time period to the microwave-free time period is 1. The operations are repeated, and the polluted soil is repaired after 1 h.
Example 3
Preparation of the sustained-release material: dissolving 1g sodium carboxymethylcellulose, adding into 100ml water for several times to obtain 1% solution, adding bentonite 10%, heating to 50 deg.C under stirring for 65 min to obtain uniform viscous solution; and (3) after the solution is cooled to room temperature, adding 6g of sodium percarbonate, 0.6g of peroxide activator Tetraacetylethylenediamine (TAED), 0.05g of stabilizer 2-hydroxyphosphonoacetic acid and 0.05g of EDTA into the solution, quickly and uniformly stirring, freeze-drying, adding 1.5g of ferrous sulfate, grinding and uniformly stirring to obtain a finished sustained-release material product 3.
And (3) repairing the toluene-polluted soil: 20g of toluene-contaminated soil to be treated with a concentration of 200mg/kg were placed in a reactor. Taking 1g of the finished sustained-release material 3, preparing a solution, and quickly adding the solution into a reactor according to a liquid-solid ratio of 2. Adjusting the pH value of the mixed environment of the soil and the water to be 4, and continuously stirring and acidizing for 10min. And (3) performing intermittent microwave treatment under the condition that the microwave power is 800W, starting the microwave for 5 seconds, pausing for 20 seconds (the ratio of the microwave time period to the microwave-free time period is 1. The operations are repeated, and the polluted soil is repaired after 1 h.
Example 4
Preparation of the sustained-release material: dissolving 1g sodium carboxymethylcellulose, adding into 33ml water for several times in small amount to obtain 3% solution, adding bentonite 2%, and heating to 70 deg.C under stirring for 45 min to obtain uniform viscous solution; and (3) after the solution is cooled to room temperature, adding 6g of sodium percarbonate, 0.6g of peroxide activator Tetraacetylethylenediamine (TAED), 0.05g of stabilizer 2-hydroxyphosphonoacetic acid and 0.05g of EDTA into the solution, quickly and uniformly stirring, freeze-drying, adding 1.8g of ferrous sulfate, grinding and uniformly stirring to obtain a finished sustained-release material 4.
And (3) repairing the toluene-polluted soil: 10g of toluene-contaminated soil to be treated having a concentration of 100mg/kg were placed in a reactor. Taking 0.8g of the slow release material finished product 4, preparing a solution, and quickly adding the solution into a reactor according to a liquid-solid ratio of 2. Adjusting the pH value of the mixed environment of the soil and the water to 5, and continuously stirring and acidizing for 10min. The intermittent microwave treatment is carried out under the condition that the microwave power is 800W, the microwave is started for 10 seconds, is suspended for 20 seconds (the ratio of the microwave time period to the microwave-free time period is 1. The operations are repeated, and the polluted soil is repaired after 1 h.
Example 5
Preparation of the sustained-release material: dissolving 1g sodium carboxymethylcellulose, adding into 50ml water for several times in small amount to obtain 2% solution, adding bentonite 5%, heating to 60 deg.C under stirring for 40 min to obtain uniform viscous solution; and (3) after the solution is cooled to room temperature, adding 6g of sodium percarbonate, 0.6g of peroxide activator Tetraacetylethylenediamine (TAED), 0.05g of stabilizer 2-hydroxyphosphonoacetic acid and 0.05g of EDTA into the solution, quickly and uniformly stirring, freeze-drying, adding 1.2g of ferrous sulfate, grinding and uniformly stirring to obtain a finished slow-release material 5.
And (3) repairing the toluene-polluted soil: 10g of toluene-contaminated soil to be treated having a concentration of 100mg/kg were placed in a reactor. Taking 0.5g of the finished sustained-release material 5, preparing a solution, and quickly adding the solution into a reactor according to a liquid-solid ratio of 1. Adjusting the pH value of the mixed environment of the soil and the water to 3, and continuously stirring and acidizing for 5min. The intermittent microwave treatment is carried out under the condition that the microwave power is 800W, the microwave is started for 10 seconds, is suspended for 30 seconds (the ratio of the microwave time period to the microwave-free time period is 1. The operations are repeated, and the polluted soil is repaired after 1 hour.
Example 6
Preparation of the sustained-release material: dissolving 1g sodium carboxymethylcellulose, adding into 100ml water for several times to obtain 1% solution, adding bentonite 10%, heating to 45 deg.C under stirring for 70 min to obtain uniform viscous solution; and (3) after the solution is cooled to room temperature, adding 6g of sodium percarbonate, 0.6g of peroxide activator Tetraacetylethylenediamine (TAED), 0.05g of stabilizer 2-hydroxyphosphonoacetic acid and 0.05g of EDTA into the solution, quickly and uniformly stirring, freeze-drying, adding 0.7g of ferrous sulfate, grinding and uniformly stirring to obtain a finished sustained-release material product 6.
And (3) repairing the toluene-polluted soil: 50g of toluene-contaminated soil to be treated having a concentration of 200mg/kg were placed in a reactor. Taking 3.5g of the finished sustained-release material 6, preparing a solution, and quickly adding the solution into the reactor according to the liquid-solid ratio of 2. Adjusting the pH value of the mixed environment of the soil and the water to be 4, and continuously stirring and acidizing for 10min. And (3) performing intermittent microwave treatment under the condition that the microwave power is 800W, starting the microwave for 5 seconds, pausing for 20 seconds (the ratio of the microwave time period to the microwave-free time period is 1. The operations are repeated, and the polluted soil is repaired after 1 h.
Example 7
Preparation of the sustained-release material: dissolving 1g sodium carboxymethylcellulose, adding into 33ml water for several times to obtain 3% solution, adding bentonite 2%, and heating to 85 deg.C under stirring for 40 min to obtain uniform viscous solution; after the solution is cooled to room temperature, 6g of sodium percarbonate, 0.6g of peroxide activator Tetraacetylethylenediamine (TAED), 0.05g of stabilizer 2-hydroxyphosphonoacetic acid and 0.05g of EDTA are added into the solution, the mixture is rapidly and uniformly stirred, after freeze drying, 1.7g of ferrous oxalate is added, and the mixture is ground and uniformly stirred to obtain a finished product 7 of the slow-release material.
And (3) repairing the toluene-polluted soil: 20g of toluene-contaminated soil to be treated having a concentration of 100mg/kg were placed in a reactor. Taking 1g of the finished sustained-release material 7, preparing a solution, and quickly adding the solution into a reactor according to a liquid-solid ratio of 1. Adjusting the pH value of the mixed environment of the soil and the water to be 4, and continuously stirring and acidizing for 5min. And (3) performing intermittent microwave treatment under the condition that the microwave power is 800W, starting the microwave for 10 seconds, pausing for 20 seconds (the ratio of the microwave time period to the microwave-free time period is 1. The operations are repeated, and the polluted soil is repaired after 1 h.
Example 8
Preparation of the sustained-release material: dissolving 1g sodium carboxymethylcellulose, adding a small amount of sodium carboxymethylcellulose into 50ml water for multiple times to obtain 2% solution, adding bentonite 8%, and heating to 80 deg.C under stirring for 45 min to obtain uniform viscous solution; and (3) after the solution is cooled to room temperature, adding 6g of sodium percarbonate, 0.6g of peroxide activator Tetraacetylethylenediamine (TAED), 0.05g of stabilizer 2-hydroxyphosphonoacetic acid and 0.05g of EDTA into the solution, quickly and uniformly stirring, freeze-drying, adding 1g of ferrous oxalate, grinding and uniformly stirring to obtain a finished sustained-release material 8.
And (3) repairing the toluene-polluted soil: 10g of toluene-contaminated soil to be treated having a concentration of 200mg/kg were placed in a reactor. Taking 1.5g of finished sustained-release material 8, preparing a solution, and quickly adding the solution into a reactor according to a liquid-solid ratio of 2. Adjusting the pH value of the soil and water mixed environment to 4, and continuously stirring and acidizing for 10min. And (3) performing intermittent microwave treatment under the condition that the microwave power is 800W, starting the microwave for 10 seconds, pausing for 30 seconds (the ratio of the microwave time period to the microwave-free time period is 1. The operations are repeated, and the polluted soil is repaired after 1 h.
Example 9
Preparation of the sustained-release material: dissolving 1g sodium carboxymethylcellulose, adding into 100ml water for several times in small amount to obtain 1% solution, adding bentonite 10%, and heating to 50 deg.C under stirring for 60 min to obtain uniform viscous solution; and (3) after the solution is cooled to room temperature, adding 6g of sodium percarbonate, 0.6g of peroxide activator Tetraacetylethylenediamine (TAED), 0.05g of stabilizer 2-hydroxyphosphonoacetic acid and 0.05g of EDTA into the solution, quickly and uniformly stirring, freeze-drying, adding 0.7g of ferrous oxalate, grinding and uniformly stirring to obtain a finished slow-release material product 9.
And (3) repairing the toluene-polluted soil: 10g of toluene-contaminated soil to be treated having a concentration of 100mg/kg were placed in a reactor. Taking 0.5g of finished sustained-release material 9, preparing a solution, and quickly adding the solution into a reactor according to a liquid-solid ratio of 2. Adjusting the pH value of the mixed environment of the soil and the water to 5, and continuously stirring and acidizing for 10min. The intermittent microwave treatment is carried out under the condition that the microwave power is 800W, the microwave is started for 5 seconds, is suspended for 20 seconds (the ratio of the microwave time period to the microwave-free time period is 1. The operations are repeated, and the polluted soil is repaired after 1 h.
Example 10
Preparation of the sustained-release material: dissolving 1g sodium carboxymethylcellulose, adding into 33ml water for several times in small amount to obtain 3% solution, adding bentonite 2%, and heating to 70 deg.C under stirring for 45 min to obtain uniform viscous solution; after the solution was cooled to room temperature, 6g of sodium percarbonate, 0.6g of the peroxide activator Tetraacetylethylenediamine (TAED): 0.05g of stabilizer 2-hydroxyphosphonoacetic acid and 0.05g of EDTA, quickly and uniformly stirring, after freeze-drying, adding 2.5g of ferrous oxalate, grinding and uniformly stirring to obtain a finished product 10 of the slow-release material.
And (3) repairing the toluene-polluted soil: 50g of toluene-contaminated soil to be treated having a concentration of 200mg/kg were placed in a reactor. Taking 3.5g of the slow release material finished product 10, preparing a solution, and quickly adding the solution into a reactor according to a liquid-solid ratio of 1. Adjusting the pH value of the soil and water mixed environment to 4, and continuously stirring and acidizing for 5min. The intermittent microwave treatment is carried out under the condition that the microwave power is 800W, the microwave is started for 10 seconds, is suspended for 20 seconds (the ratio of the microwave time period to the microwave-free time period is 1. The operations are repeated, and the polluted soil is repaired after 1 h.
Example 11
Preparation of the sustained-release material: dissolving 1g sodium carboxymethylcellulose, adding a small amount of sodium carboxymethylcellulose into 50ml water for multiple times to obtain 2% solution, adding bentonite 5%, and heating to 60 deg.C for 50 min under continuous stirring to obtain uniform viscous solution; after the solution is cooled to room temperature, 6g of sodium percarbonate, 0.6g of peroxide activator Tetraacetylethylenediamine (TAED), 0.05g of stabilizer 2-hydroxyphosphonoacetic acid and 0.05g of EDTA are added into the solution, the mixture is rapidly and uniformly stirred, after freeze drying, 1.2g of ferrous oxalate is added, and the mixture is ground and uniformly stirred, so that a finished product 11 of the slow-release material is obtained.
And (3) repairing the toluene-polluted soil: 10g of toluene-contaminated soil to be treated having a concentration of 100mg/kg were placed in a reactor. Taking 0.5g of the finished sustained-release material 11, preparing a solution, and quickly adding the solution into a reactor according to a liquid-solid ratio of 2. Adjusting the pH value of the mixed environment of the soil and the water to be 4, and continuously stirring and acidizing for 10min. And (3) performing intermittent microwave treatment under the condition that the microwave power is 800W, starting the microwave for 10 seconds, pausing for 30 seconds (the ratio of the microwave time period to the microwave-free time period is 1. The operations are repeated, and the polluted soil is repaired after 1 h.
Example 12
Preparation of the sustained-release material: dissolving 1g sodium carboxymethylcellulose, adding a small amount of sodium carboxymethylcellulose into 100ml water for multiple times to obtain 1% solution, adding bentonite 10%, and heating to 45 deg.C under stirring for 60 min to obtain uniform viscous solution; after the solution is cooled to room temperature, 6g of sodium percarbonate, 0.6g of peroxide activator Tetraacetylethylenediamine (TAED), 0.05g of stabilizer 2-hydroxyphosphonoacetic acid and 0.05g of EDTA are added into the solution, the mixture is rapidly and uniformly stirred, after freeze drying, 1g of ferrous oxalate is added, and the mixture is ground and uniformly stirred, so that the finished sustained-release material 12 is obtained.
And (3) repairing the toluene-polluted soil: 10g of toluene-contaminated soil to be treated having a concentration of 100mg/kg were placed in a reactor. Taking 0.8g of the finished sustained-release material 12, preparing a solution, and quickly adding the solution into the reactor according to the liquid-solid ratio of 2. Adjusting the pH value of the mixed environment of the soil and the water to 3, and continuously stirring and acidizing for 10min. The intermittent microwave treatment is carried out under the condition that the microwave power is 800W, the microwave is started for 5 seconds, is suspended for 20 seconds (the ratio of the microwave time period to the microwave-free time period is 1. The operations are repeated, and the polluted soil is repaired after 1 h.
Claims (5)
1. A method for promoting Fenton reaction to repair organic contaminated soil by using a microwave slow-release material is characterized by comprising the following steps:
step S1: dissolving 10 parts of sodium carboxymethylcellulose in water to prepare a 1-3% solution, adding 2-10% of bentonite, heating to 45-85 ℃ for 40-70 minutes to form a uniform viscous solution;
step S2: adding 60 parts of sodium percarbonate, 6 parts of peroxide activator Tetraacetylethylenediamine (TAED), 0.5 part of stabilizer 2-hydroxyphosphonoacetic acid and 0.5 part of EDTA into the solution, quickly and uniformly stirring, filtering or centrifugally separating, drying until the quality is constant, adding 7-25 parts of ferrous sulfate or ferrous oxalate, and uniformly stirring to obtain a finished slow-release material;
and step S3: the sodium carboxymethylcellulose and the bentonite are in cross-linking with the sodium percarbonate to prevent the sodium percarbonate from being decomposed inefficiently due to too fast speed, so that the speed of releasing the hydrogen peroxide is slow and controllable, the sodium percarbonate and Fe (II) components in the material form a Fenton reagent, and the Fe (II) catalyzes the hydrogen peroxide to generate hydroxyl radicals, thereby realizing the degradation of pollutants;
and step S4: the stabilizers 2-hydroxyphosphonoacetic acid and EDTA are used to chelate the heavy metal ions in the reaction medium, preventing them from catalyzing the decomposition reaction of sodium percarbonate.
Step S5: and (5) repairing.
2. The method for restoring the organic contaminated soil by the aid of the microwave sustained-release material for promoting fenton reaction according to claim 1, wherein the microwaves in the step S5 have the effects of controlling the sodium percarbonate in the sustained-release material to release hydrogen peroxide, promoting desorption and solubilization of soil pesticides, improving the contact effect of the pollutants and the oxidant, creating favorable conditions for the oxidant to fully degrade the pollutants, and reducing non-targeted oxidation processes such as soil organic matter oxidation and the like.
3. The method for remediating organic contaminated soil by promoting fenton reaction by using the microwave sustained-release material according to claim 1, wherein the peroxide activator Tetraacetylethylenediamine (TAED) in the step S2 is used for activating peroxide to release nascent oxygen at normal temperature, so that the oxidation efficiency is improved.
4. The method for restoring organic contaminated soil by promoting Fenton's reaction through microwave sustained-release materials according to claim 1, wherein in the method, the method
The oxidant is sodium percarbonate, the catalyst is ferrous sulfate or ferrous oxalate, the cross-linking agent is sodium carboxymethylcellulose, the mineral matrix is bentonite, the peroxide activator is Tetraacetylethylenediamine (TAED), and the stabilizer is 2-hydroxyphosphonoacetic acid.
5. The method for remediating organic contaminated soil by promoting fenton' S reaction by using the microwave sustained-release material according to claim 1, wherein the step S5 comprises the following substeps:
s51: putting the organic contaminated soil to be treated into a reactor, wherein the mass of the soil is 10-50 g.
S52: preparing a slow-release material aqueous solution, and stirring and mixing the slow-release material aqueous solution with the organic contaminated soil, wherein the liquid-solid ratio is 1.
S53: adjusting the pH value of the soil and water mixed environment to 3-5, and carrying out acidification treatment for 5-10 min.
S54: and intermittently emitting microwaves under the condition that the microwave power is 300-850W, wherein the microwave time period and the microwave-free time period are 1.
S55: under the condition of the intermittent microwave, the treatment time is 30-300 s, the standing reaction is 0.2-1 h to form a period, and the polluted soil can be repaired in a plurality of periods.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105668689A (en) * | 2016-04-11 | 2016-06-15 | 华东理工大学 | Multifunctional slow-release restoration agent applied to underground water in-situ restoration |
| CN106623382A (en) * | 2016-12-22 | 2017-05-10 | 常州大学 | Method for repairing organochlorine pesticide-polluted soil through microwave-enhanced sodium percarbonate |
| CN110002571A (en) * | 2019-04-10 | 2019-07-12 | 清华大学 | For the controlled release composition of organic contamination underground water in situ chemical oxidation, preparation method and application |
| CN110615518A (en) * | 2019-05-07 | 2019-12-27 | 中冶华天工程技术有限公司 | Fenton reaction ferrous iron slow release granule |
| CN113087120A (en) * | 2021-05-11 | 2021-07-09 | 常州绿玛特建筑科技有限公司 | Oxidation repair slow-release material applied to benzene series polluted water body and preparation method thereof |
-
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105668689A (en) * | 2016-04-11 | 2016-06-15 | 华东理工大学 | Multifunctional slow-release restoration agent applied to underground water in-situ restoration |
| CN106623382A (en) * | 2016-12-22 | 2017-05-10 | 常州大学 | Method for repairing organochlorine pesticide-polluted soil through microwave-enhanced sodium percarbonate |
| CN110002571A (en) * | 2019-04-10 | 2019-07-12 | 清华大学 | For the controlled release composition of organic contamination underground water in situ chemical oxidation, preparation method and application |
| CN110615518A (en) * | 2019-05-07 | 2019-12-27 | 中冶华天工程技术有限公司 | Fenton reaction ferrous iron slow release granule |
| CN113087120A (en) * | 2021-05-11 | 2021-07-09 | 常州绿玛特建筑科技有限公司 | Oxidation repair slow-release material applied to benzene series polluted water body and preparation method thereof |
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