CN113751492B - Method for repairing organic contaminated soil by using magnetic lignin hydrogel to activate persulfate - Google Patents
Method for repairing organic contaminated soil by using magnetic lignin hydrogel to activate persulfate Download PDFInfo
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- CN113751492B CN113751492B CN202111062031.6A CN202111062031A CN113751492B CN 113751492 B CN113751492 B CN 113751492B CN 202111062031 A CN202111062031 A CN 202111062031A CN 113751492 B CN113751492 B CN 113751492B
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- B09C1/08—Reclamation of contaminated soil chemically
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Abstract
The invention discloses a method for repairing organic contaminated soil by using magnetic lignin hydrogel to activate persulfate, and belongs to the technical field of degradation of environmental organic pollutants. The invention takes nanometer zero-valent iron-nickel bimetal as a magnetic source, and the nanometer zero-valent iron-nickel bimetal is mixed with lignin hydrogel to prepare the magnetic lignin hydrogel which is used for activating persulfate to repair organic contaminated soil, wherein the removal rate of bisphenol A in the soil can reach more than 88%. The reaction condition of the invention can be carried out at normal temperature and normal pressure, and the invention has good effect of degrading organic pollutants in soil and is environment-friendly. The applied magnetic lignin hydrogel does not produce secondary pollution, does not need additional energy such as light, electricity, heat, ultrasound and the like, saves energy, has strong oxidation resistance, can still keep high-efficiency catalytic performance after being exposed in the air for a long time, is simple and convenient to operate, and is easy to popularize. Therefore, the method has good application prospect in the field of organic contaminated soil remediation.
Description
Technical Field
The invention belongs to the technical field of degradation of environmental organic pollutants, and particularly relates to a method for repairing organic polluted soil by using magnetic lignin hydrogel to activate persulfate.
Background
Along with the development of industry and agriculture, the popularization of sewage field return irrigation engineering and the like, the organic contaminated soil area is wider and wider. In recent years, the degree of organic pollution of soils around cities and industrial areas has increased due to the acceleration of industrialization and urbanization. According to the 2014 'national soil pollution condition survey bulletin', the national industrial enterprises are moved to leave over 50 thousands of severely polluted sites. The organic pollutants in the soil are various, such as plastic plasticizers, polychlorinated biphenyl, polycyclic aromatic hydrocarbons, organic pesticides and the like, generally have the toxicity of carcinogenesis, mutagenesis, teratogenesis and the like, and have the characteristics of environmental persistence, biological accumulation and the like. Organic pollutants in soil can enter a plant ecosystem and a water environment through a food chain and a food net, and seriously threatens the health of people and livestock and the safety of drinking water. When the traditional biological treatment technology is used for repairing the organic polluted soil, the defects of long repair period, poor repair effect and the like are often shown.
The persulfate-based advanced oxidation technology (PS-AOPs) has the advantages of strong oxidation capacity, small selectivity, high reaction rate, high treatment efficiency and the like, and has certain advantages when organic pollutants in the environment are degraded. Compared with the traditional Fenton oxidation technology, the method has the advantages that the sulfate radical generated by activating persulfate has higher oxidation-reduction potential and longer half life, which means that the sulfate radical can stay in the system for longer time and can be contacted with target pollutants for a long distance so as to degrade the pollutants more thoroughly. In addition, the solid persulfate is more convenient to transport and store; in recent years, PS-AOPs have been paid close attention by researchers and engineers in the field of remediation of organically contaminated soil.
The traditional persulfate activation mode mainly comprises light energy, heat energy or electric energy and the like, but the application of the persulfate in an actual field is greatly limited due to the consumption of energy; the transition metal-based homogeneous phase material has a high persulfate activation rate, so that the phenomenon of self-quenching of free radicals is easily caused, and the problems of secondary pollution of metal ions and the like also exist. Therefore, the development of an environmentally friendly and efficient heterogeneous catalytic material is one of the research hotspots in academic and engineering circles at present.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a method for repairing organic contaminated soil by using magnetic lignin hydrogel to activate persulfate.
The invention takes nanometer zero-valent iron-nickel bimetal as a magnetic source, and the nanometer zero-valent iron-nickel bimetal is mixed with lignin hydrogel to prepare the magnetic lignin hydrogel which is used for activating persulfate to repair organic contaminated soil. The invention aims to solve the problems that zero-valent metals represented by nano zero-valent iron and nickel are easy to oxidize and difficult to store in the air and the like, and provides a method for repairing organic contaminated soil by using magnetic lignin hydrogel activated persulfate. Compared with the pure nanometer zero-valent iron-nickel bimetallic material, the material of the invention has the advantages of good degradation effect, low cost, simple and convenient operation, easy storage, capability of effectively slowing down the oxidation speed of the nanometer zero-valent iron-nickel bimetallic material in the air and the like.
The purpose of the invention is realized by the following technical scheme:
a method for repairing organic contaminated soil by using magnetic lignin hydrogel activated persulfate comprises the following steps:
and (2) adding persulfate into the organic polluted soil at normal temperature, uniformly mixing, adding the magnetic lignin hydrogel as a catalyst, and then carrying out oscillation reaction, thereby effectively degrading the organic pollutants in the soil. Wherein, sampling, testing and analyzing are carried out at intervals, and the removal efficiency of the pollutants is calculated.
Preferably, the persulfate may be at least one of sodium persulfate, ammonium persulfate, and potassium persulfate.
Preferably, the magnetic lignin hydrogel is prepared by mixing nano zero-valent iron-nickel bimetal serving as a magnetic source with the lignin hydrogel.
Preferably, the preparation method of the magnetic lignin hydrogel comprises the following steps:
(1) weighing acrylamide, lignosulfonate, maleic anhydride and N, N-methylene bisacrylamide, dissolving in water, and stirring until the acrylamide, the lignosulfonate, the maleic anhydride and the N, N-methylene bisacrylamide are completely dissolved; adjusting the pH value to 6.0-8.0 (preferably to 6.0); adding persulfate, stirring for dissolving, adding tetramethylethylenediamine, fully stirring, standing, and drying; drying, grinding and sieving to obtain lignin hydrogel;
(2) then weighing lignin hydrogel, ferric salt, nickel salt and polyethylene glycol, dissolving in ethanol water solution, stirring for dissolving, and dropwise adding NaBH in nitrogen atmosphere 4 And (3) centrifuging the solution to collect a solid, washing the solid with ethanol and water, and performing vacuum freeze drying to obtain the magnetic lignin hydrogel.
In the step (1), the lignosulfonate may be at least one of sodium lignosulfonate, calcium lignosulfonate and magnesium lignosulfonate.
In the step (1), the molecular weight of the lignosulfonate is 5000-30000; further 5000 to 20000; and still further 8000. If the molecular weight is below this range, the strength of the material is lowered.
In the step (1), the water may be one of deionized water, pure water and ultrapure water.
In the step (1), the stirring may be one of magnetic stirring and mechanical stirring.
In the step (1), the persulfate may be one of potassium persulfate and sodium persulfate.
In the step (1), the mass ratio of acrylamide, lignosulfonate, maleic anhydride, N-methylene bisacrylamide and water is as follows: 1.00-10.00 g: 0.3-0.6 g: 1.0-2.0 g: 0.01-0.1 g: 20.0-40.0 g; further 3.00 g: 0.32 g: 1.33 g: 0.02 g: 20 g.
In the step (1), the mass ratio of the lignosulfonate to the persulfate is as follows: 0.3-0.6 g: 0.05-0.15 g; further 0.32 g: 0.05 g;
in the step (1), the ratio of the lignosulfonate to the tetramethylethylenediamine is as follows: 0.3-0.6 g: 40-100 μ L; further 0.3 to 0.6 g: 40-80 mu L; still further 0.32 g: 40 mu L of the solution; if the amount of tetramethylethylenediamine added is less than this range, the material cannot be prepared.
In the step (1), drying is carried out at the temperature of 50-80 ℃; further at 60 ℃.
In the step (1), the screening is carried out, wherein the mesh number is 60-200 meshes; further 100 meshes.
In the step (2), the ferric salt comprises one of ferrous sulfate, ferric chloride and ferric nitrate; the nickel salt comprises one of nickel nitrate and nickel sulfate.
In the step (2), the molecular weight of the polyethylene glycol is 1000-20000; further 2000 to 6000.
In the step (2), the molar ratio of the ferric salt to the nickel salt is 4-5: 2-1; further 5: 1.
in the step (2), the lignin hydrogel, the iron salt and the nickel salt are reduced to generate Fe according to the specific requirement of the iron salt and the nickel salt 0 、Ni 0 Is calculated. Specifically, the lignin hydrogel: fe 0 Ni 0 The mass ratio of (A) is as follows: 0.2-1: 1; further 0.2 to 0.8: 1; further, 0.2: 1.
in the step (2), the mass-to-volume ratio (g/mL) of the lignin hydrogel to the ethanol aqueous solution is 0.271 g: 50-100 mL; further 0.271 g: 50 mL.
In the step (2), the sum of ferric salt and nickel salt is reacted with NaBH 4 The molar ratio of (iron salt + nickel salt): NaBH 4 1: 1-4; further 1: 2.
in the step (2), the volume ratio of ethanol to water in the ethanol aqueous solution is 40-70: 60-30 parts of; further 50-70: 50-30; further 70: 30.
in the step (2), the NaBH is 4 The concentration of the solution is 0.5 mol/L-2.0 mol/L; further 1.0mol/L to 1.5 mol/L.
In the step (2), the ethanol aqueous solution and NaBH 4 The volume ratio of the solution is 1: 1-2, further 1: 1.
preferably, the concentration of the organic pollutants in the soil is 5-1000 mg/kg; more preferably 500 mg/kg.
Preferably, the organic contaminant is bisphenol a.
Preferably, the concentration of the persulfate in the soil reaction system is 2.5-50 g/kg; further 2.5 to 20 g/kg.
Preferably, the concentration of the magnetic lignin hydrogel in the soil reaction system is 2.5-50 g/kg; more preferably 2.5 to 5 g/kg.
More preferably, the mass ratio of the bisphenol a, the persulfate and the magnetic lignin hydrogel in the soil reaction system is 0.001-0.2: 0.5-10: 1; further 0.1: 4: 1.
preferably, the oscillation reaction time is 10-150 min; further preferably 10-15 min; more preferably 15 min.
Preferably, the magnetic lignin hydrogel in the method can be fully exposed in the air for 7 days to be oxidized, and bisphenol A in the soil can still be efficiently degraded.
The organic contaminated soil mainly refers to organic contaminated soil generated by leakage of industrial and agricultural organic pollutants.
Adding water after the persulfate is added to help the soil to form a water-rich state so as to be beneficial to uniform stirring; if the water content of the soil is high (such as bottom mud), water can not be added.
Preferably, the normal temperature is 15-40 ℃.
The mechanism of the invention is as follows:
according to the invention, the magnetic lignin hydrogel is used as a heterogeneous catalysis material, so that persulfate can be effectively activated to generate sulfate radicals and hydroxyl radicals, and organic pollutants in soil can be efficiently degraded. The material is easy to prepare, and has the advantages of high catalytic effect, strong oxidation resistance, high performance-price ratio, easy storage, difficult deterioration and the like. At present, researches or patents for degrading organic pollutants in soil by using the magnetic lignin hydrogel to activate persulfate to generate free radicals are not found. Meanwhile, in the previous research, a load-based nano zero-valent metal material is available, organic pollutants in soil are degraded by efficiently activating persulfate, and the material can be exposed in the air for a long time without affecting the efficient catalytic performance of the material. Therefore, the invention provides a method for repairing organic contaminated soil by using magnetic lignin hydrogel to activate persulfate, which can effectively degrade organic pollutants in soil.
Compared with the prior art, the invention has the following advantages and effects:
(1) the invention provides a novel remediation method applied to organic contaminated soil, and particularly relates to a method for degrading organic pollutants in soil by adding magnetic lignin hydrogel and persulfate into the contaminated soil and uniformly stirring.
(2) The magnetic lignin hydrogel applied in the invention can not generate secondary pollution, and simultaneously does not need to provide extra energy such as light, electricity, heat, ultrasound and the like, thereby saving energy, and having simple and convenient operation and easy popularization.
(3) The magnetic lignin hydrogel applied in the invention can solve the problem that nano zero-valent metal is easy to oxidize in the air, has strong oxidation resistance, and can still retain the high-efficiency catalytic performance after being exposed in the air for a long time.
(4) The method disclosed by the invention utilizes the magnetic lignin hydrogel as an activating agent and the persulfate as an oxidizing agent to degrade single or composite organic pollutants in the soil, wherein the removal rate of bisphenol A in the soil can reach more than 88%. The reaction condition of the invention can be carried out at normal temperature and normal pressure, has good degradation effect on organic pollutants in soil, is environment-friendly, and has good application prospect in the field of organic polluted soil remediation.
Drawings
FIG. 1 is an XRD pattern of the magnetic lignin hydrogel prepared in example 1 (lignin hydrogel: Fe-Ni mass ratio of 0.2: 1).
FIG. 2 is a scanning electron microscope image of the magnetic lignin hydrogel prepared in example 1 (lignin hydrogel: Fe-Ni mass ratio: 0.2: 1).
FIG. 3 is an XRD pattern of the magnetic lignin hydrogel prepared in example 5 (lignin hydrogel: Fe-Ni mass ratio of 0.8: 1).
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
The embodiment of the invention takes bisphenol A as a typical organic pollutant, and meanwhile, the bisphenol A is also a typical organic pollutant which is difficult to biodegrade. It is a raw material of various chemical products in industry, and is widely used for synthesizing materials such as polycarbonate, epoxy resin and the like. The trace of the disease can be seen in life and production. In the organic contaminated soil, it was studied as a target contaminant in the following examples as a typical organic contaminant. Such contaminants are merely illustrative of the invention, but the process is not limited to such contaminants.
Example 1
A preparation method of a magnetic lignin hydrogel comprises the following steps:
weighing 3.00g of acrylamide, 0.32g of sodium lignosulfonate (molecular weight of 8000), 1.33g of maleic anhydride and 0.02g of N, N-methylene bisacrylamide according to a certain proportion, dissolving in 20mL of pure water, and magnetically stirring until the acrylamide, the sodium lignosulfonate and the N, N-methylene bisacrylamide are completely dissolved; adjusting the pH to 6.0; adding 0.05g of potassium persulfate, stirring for dissolving, finally adding 40 mu L of tetramethylethylenediamine, fully stirring, standing, solidifying and drying at 60 ℃; and grinding the dried lignin hydrogel by using a mortar, and sieving by using a 100-mesh sieve to obtain the lignin hydrogel. Weighing 0.271g of lignin hydrogel and 0.02mol of FeSO 4 .7H 2 O、0.004mol NiSO 4 .6H 2 O, 0.5g polyethylene glycol (molecular weight 2000), dissolved in 50mL aqueous ethanol (ethanol: water: 70: 30), dissolved with stirring, and 50mL 1M NaBH was added dropwise under nitrogen atmosphere 4 And finally centrifuging the solution, washing the solution by using ethanol and water, and performing vacuum freeze drying to obtain the magnetic lignin hydrogel which is recorded as LH @ nZVI/Ni.
The XRD pattern of the prepared magnetic lignin hydrogel is shown in figure 1, and the scanning electron micrograph is shown in figure 2.
As can be seen from the graphs in FIGS. 1 and 2, the nano zero-valent iron-nickel bimetallic (nZVI/Ni) is successfully loaded on the Lignin Hydrogel (LH), and has a better structure. By using the magnetic lignin hydrogel, persulfate is activated to generate free radicals to degrade organic pollutants in soil, and no related literature or patent report exists. Therefore, the magnetic lignin hydrogel/persulfate system can be used for repairing the organic contaminated soil.
Example 2
Adding sodium persulfate into bisphenol A contaminated soil with the mass content of 500mg/kg to enable the concentration of the sodium persulfate to be 20g/kg, adding the magnetic lignin hydrogel of the embodiment 1 to enable the material concentration to be 5g/kg, adding a proper amount of water, and stirring for reaction, wherein the removal rate can reach over 88% within 15 min. However, when only sodium persulfate or only the magnetic lignin hydrogel was added, the removal rate of the contaminants was less than 3%.
Example 3
In the same manner as in example 2, the magnetic lignin hydrogel of example 1 was sufficiently exposed to air and oxidized for 7 days, sodium persulfate was added to bisphenol a contaminated soil having a mass content of 500mg/kg so that the sodium persulfate concentration was 20g/kg, the magnetic lignin hydrogel oxidized by exposure to air was added so that the material concentration was 5g/kg, and an appropriate amount of water was added and the reaction was stirred, so that the removal rate was maintained at 86% or more within 15 min.
Example 4
Preparation of lignin hydrogel by changing the synthesis method of the material, reference example 1; specifically, 0.271g of lignin hydrogel and 0.02mol of FeSO were weighed 4 .7H 2 O、0.004mol NiSO 4 .6H 2 Dissolving 0.5g of polyethylene glycol (molecular weight 2000) in 50mL of ethanol water (ethanol: water: 70: 30), magnetically stirring for 24 hours to enable the lignin hydrogel to fully adsorb iron and nickel ions, then centrifuging, collecting the lignin hydrogel, and washing with ultrapure water. Soaking the lignin hydrogel into 50mL of 1M NaBH 4 Stirring the solution, introducing nitrogen for 1h, centrifuging to collect solid, washing with ethanol and water, and vacuum freeze-drying. Soil reaction system reference example 2. The material prepared by the method has no magnetism, can not effectively activate persulfate to degrade bisphenol compounds in soil, and has the pollutant removal efficiency lower than 3 percent.
Example 5
In the same way as in example 1, by changing the lignin hydrogel with iron nickel (Fe) 0 Ni 0 ) The loading ratio of (3) and setting the lignin hydrogel: the mass ratio of iron to nickel is 0.2: 1. 0.4: 1. 0.6: 1. 0.8: 1. 1: 1; wherein the molar ratio of iron to nickel is kept to be 5: 1; specifically, the gradient pure iron-nickel (Fe) needs to be generated theoretically by calculation 0 Ni 0 ) The mass of the iron salt and the nickel salt required by the mass. Wherein, for the loading proportion of the lignin hydrogel: the iron and nickel content is 0.8: 1, the XRD test shows that the spectrum has no obvious metallic iron and nickel peaks, as shown in figure 3. The lignin hydrogel can effectively wrap the nano zero-valent iron and nickel under the loading proportion,the effects of dispersing and protecting the nano zero-valent iron-nickel particles are achieved.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such modifications are intended to be included in the scope of the present invention.
Claims (10)
1. A method for repairing organic contaminated soil by using magnetic lignin hydrogel to activate persulfate is characterized by comprising the following steps: the method comprises the following steps:
at normal temperature, adding persulfate into the organic contaminated soil, uniformly mixing, adding magnetic lignin hydrogel serving as a catalyst, and then carrying out oscillation reaction, thereby effectively degrading the organic contaminants in the soil;
the magnetic lignin hydrogel is prepared by mixing nano zero-valent iron-nickel bimetal serving as a magnetic source with lignin hydrogel;
the preparation method of the magnetic lignin hydrogel comprises the steps of weighing lignin hydrogel, ferric salt, nickel salt and polyethylene glycol, dissolving the lignin hydrogel, ferric salt, nickel salt and polyethylene glycol in ethanol water solution, stirring the mixture to dissolve the lignin hydrogel, and dropwise adding NaBH in the nitrogen atmosphere 4 And (3) centrifuging the solution, collecting a solid, washing the solid by using ethanol and water, and performing vacuum freeze drying to obtain the magnetic lignin hydrogel.
2. The method of claim 1, wherein:
the concentration of the organic pollutants in the soil is 5-1000 mg/kg;
the organic pollutant is bisphenol A;
the concentration of persulfate in the soil reaction system is 2.5-50 g/kg;
the concentration of the magnetic lignin hydrogel in the soil reaction system is 2.5-50 g/kg;
the mass ratio of the bisphenol A to the persulfate to the magnetic lignin hydrogel in the soil reaction system is 0.001-0.2: 0.5-10: 1.
3. the method of claim 2, wherein:
the concentration of the organic pollutants in the soil is 500 mg/kg;
the concentration of persulfate in the soil reaction system is 2.5-20 g/kg;
the concentration of the magnetic lignin hydrogel in the soil reaction system is 2.5-5 g/kg;
the mass ratio of bisphenol A, persulfate and magnetic lignin hydrogel in the soil reaction system is 0.1: 4: 1.
4. the method of claim 1, wherein:
the persulfate is at least one of sodium persulfate, ammonium persulfate and potassium persulfate;
the oscillation reaction time is 10-150 min.
5. The method of claim 1, wherein:
the organic contaminated soil mainly refers to organic contaminated soil generated by leakage of industrial and agricultural organic pollutants;
adding water after the persulfate is added to help the soil to form a water-rich state so as to be beneficial to uniform stirring;
the temperature at the normal temperature is 15-40 ℃.
6. The method according to any one of claims 1 to 5, wherein:
the preparation method of the magnetic lignin hydrogel comprises the following steps:
(1) weighing acrylamide, lignosulfonate, maleic anhydride and N, N-methylene bisacrylamide, dissolving in water, and stirring until the acrylamide, the lignosulfonate, the maleic anhydride and the N, N-methylene bisacrylamide are completely dissolved; adjusting the pH value to 6.0-8.0; adding persulfate, stirring for dissolving, adding tetramethylethylenediamine, fully stirring, standing, and drying; drying, grinding and sieving to obtain lignin hydrogel;
(2) however, the device is not suitable for use in a kitchenThen weighing lignin hydrogel, ferric salt, nickel salt and polyethylene glycol, dissolving in ethanol water solution, stirring for dissolving, and dropwise adding NaBH under nitrogen atmosphere 4 And (3) centrifuging the solution to collect a solid, washing the solid with ethanol and water, and performing vacuum freeze drying to obtain the magnetic lignin hydrogel.
7. The method of claim 6, wherein:
in the step (1), the mass ratio of acrylamide, lignosulfonate, maleic anhydride, N-methylene bisacrylamide and water is as follows: 1.00-10.00 g: 0.3-0.6 g: 1.0-2.0 g: 0.01-0.1 g: 20.0-40.0 g;
in the step (1), the mass ratio of the lignosulfonate to the persulfate is as follows: 0.3-0.6 g: 0.05-0.15 g;
in the step (1), the ratio of the lignosulfonate to the tetramethylethylenediamine is as follows: 0.3-0.6 g: 40-100 μ L.
8. The method of claim 6, wherein:
in the step (1), the lignosulfonate is at least one of sodium lignosulfonate, calcium lignosulfonate and magnesium lignosulfonate;
in the step (1), the molecular weight of the lignosulfonate is 5000-30000;
in the step (1), the water is one of deionized water, pure water and ultrapure water;
in the step (1), the stirring is one of magnetic stirring and mechanical stirring;
in the step (1), the persulfate is one of potassium persulfate and sodium persulfate;
in the step (1), drying is carried out at the temperature of 50-80 ℃;
in the step (1), the sieve is used for sieving the materials, and the mesh number is 60-200 meshes.
9. The method of claim 6, wherein:
in the step (2), the molar ratio of the ferric salt to the nickel salt is 4-5: 2-1;
in the step (2), the lignin hydrogel: fe 0 Ni 0 The mass ratio of (A) to (B) is as follows: 0.2-1: 1;
in the step (2), the mass-to-volume ratio of the lignin hydrogel to the ethanol aqueous solution is 0.271 g: 50-100 mL;
in the step (2), the sum of ferric salt and nickel salt is reacted with NaBH 4 The molar ratio of (iron salt + nickel salt): NaBH 4 ＝1：1～4。
10. The method of claim 6, wherein:
in the step (2), the ferric salt comprises one of ferrous sulfate, ferric chloride and ferric nitrate; the nickel salt comprises one of nickel nitrate and nickel sulfate;
in the step (2), the molecular weight of the polyethylene glycol is 1000-20000;
in the step (2), the volume ratio of ethanol to water in the ethanol aqueous solution is 40-70: 60-30 parts of;
in the step (2), the NaBH is 4 The concentration of the solution is 0.5 mol/L-2.0 mol/L;
in the step (2), the ethanol aqueous solution and NaBH 4 The volume ratio of the solution is 1: 1 to 2.
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