CN111014275B - Heavy metal soil remediation agent and application thereof - Google Patents
Heavy metal soil remediation agent and application thereof Download PDFInfo
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- CN111014275B CN111014275B CN201911320309.8A CN201911320309A CN111014275B CN 111014275 B CN111014275 B CN 111014275B CN 201911320309 A CN201911320309 A CN 201911320309A CN 111014275 B CN111014275 B CN 111014275B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
- B09C1/08—Reclamation of contaminated soil chemically
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- C09K17/40—Soil-conditioning materials or soil-stabilising materials containing mixtures of inorganic and organic compounds
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Abstract
The invention provides a heavy metal soil remediation agent, which consists of a heavy metal adsorption fixing agent and a soil conditioning agent, and the mass fraction ratio of the heavy metal adsorption fixing agent to the soil conditioning agent is 10: 1-10 parts of heavy metal adsorption fixing agent, wherein the heavy metal adsorption fixing agent comprises 100 parts of basic iron oxide-graphene oxide gel powder and 1-100 parts of iron oxide-polypyrrole composite particles, the soil conditioning agent is one or more of a pH conditioning agent, a loosening agent, a mineral source conditioning agent and a water-retaining agent, and the heavy metal soil repairing agent is directly applied to polluted soil.
Description
Technical Field
The invention relates to the technical field of heavy metal pollution remediation, in particular to a heavy metal soil remediation agent and application thereof.
Background
The inorganic pollutants in the soil are relatively outstanding in heavy metals, mainly caused by human factors such as mining, waste gas emission, sewage irrigation, use of products with excessive heavy metals and the like, and the heavy metals cannot be decomposed by soil microorganisms and are easy to accumulate and are converted into methyl compounds with higher toxicity, even some of the heavy metals are accumulated in a human body through a food chain, the repentance of the heavy metals into the human body causes the human body to be disordered and seriously harms the human body health, so that effective measures are taken to improve the heavy metal pollution of the soil.
The existing methods for repairing soil heavy metal can be divided into three types: the method is characterized by comprising a physical method, a chemical method and a biological method, wherein the physical method comprises a deep ploughing method, a soil-bearing method and the like, the chemical method comprises a leaching method, a passivation method and the like, the biological method comprises a plant restoration method and a microorganism restoration method, wherein the passivation method is realized by adding a restoration agent to realize passivation or fixation, and the method becomes a soil heavy metal pollution restoration technology with better prospect due to the advantages of simple and convenient operation, short restoration period and the like, but the current soil restoration agent still has some defects, such as secondary heavy metal pollution, single component type of the restoration agent, insufficient restoration efficiency, restoration stability problem and the like.
Disclosure of Invention
Aiming at the problems, the invention provides a heavy metal soil remediation agent.
The purpose of the invention is realized by adopting the following technical scheme:
a heavy metal soil remediation agent comprises a heavy metal adsorption fixing agent and a soil conditioning agent, and the mass ratio of the heavy metal adsorption fixing agent to the soil conditioning agent is 10: 1-10, wherein the heavy metal adsorption fixing agent is basic iron oxide-graphene oxide gel powder, and the soil conditioner is one or more of a pH regulator, a loosening agent, a mineral source conditioner and a water-retaining agent;
preferably, the heavy metal adsorption fixing agent consists of basic iron oxide-graphene oxide gel powder and iron oxide-polypyrrole composite particles, and the relative mass ratio of the basic iron oxide-graphene oxide gel powder to the iron oxide-polypyrrole composite particles is 100: 1-100;
preferably, the iron oxide-polypyrrole composite particles are sulfydryl modified iron oxide-polypyrrole composite particles;
preferably, the heavy metal used as the heavy metal adsorption fixing agent is one or more of Cr, Cd, Hg and Pb;
preferably, the pH regulator is one or more of calcium carbonate, calcium sulfate, magnesium hydroxide, oxalic acid and ferrous sulfate;
preferably, the bulking agent is one or more of talcum powder, fly ash, medical stone, phosphate rock powder and apatite;
preferably, the mineral source conditioner is one or more of bentonite, diatomite, sepiolite and vermiculite;
preferably, the water-retaining agent is one or more of chitosan, polyacrylic acid, polyvinyl alcohol and polyethylene glycol;
preferably, the preparation of the alkali iron oxide-graphene oxide gel powder comprises the following steps:
(a) preparation of basic iron oxide
Preparing basic iron oxide by solid-phase method and using FeCl3·6H2Ball milling with O as iron source and urea as hydroxyl source in ball mill3·6H2The molar ratio of O to urea is 1:4-6, the ball milling time is 1-3h, after the ball milling is finished, the product is aged for 12-24h in a water bath at 50-70 ℃, and then the product is washed by distilled water and freeze-dried to prepare basic ferric oxide;
(b) preparation of gel powder
Ultrasonically dispersing graphene oxide in distilled water, wherein the solid-liquid ratio is 1 g: 1L, adding 20wt.% of hydrazine hydrate solution accounting for 20-30% of the volume of the system, adding 0.8-1 times of basic iron oxide in mass of solid phase material, uniformly mixing, transferring to a hydrothermal reaction kettle, carrying out hydrothermal temperature of 200 ℃ and 220 ℃, reacting for 6-10h, soaking with distilled water after the reaction is finished and cooled, changing water every 12h until the solution is neutral to obtain hydrogel, and freeze-drying, drying and crushing;
preferably, the preparation method of the sulfydryl modified iron oxide-polypyrrole composite particles comprises the following steps: nano Fe2O3Ultrasonically dispersing in distilled water, wherein the solid-liquid ratio is 2 g: 1L, adding polyvinylpyrrolidone with the mass of 0.2-0.3 times of that of a solid phase material, mechanically stirring, adding pyrrole with the volume of 0.05% of the system volume, continuously stirring, dropwise adding 4.0g/L ferric chloride solution with the volume of 20-30% of the system volume, continuously stirring for 5h, centrifuging, washing with deionized water and ethanol respectively, and mixing the product according to the material-liquid ratio of 1: 5-20, adding ethanol, magnetically stirring in a water bath at a constant temperature of 50 ℃, adding 0.5-0.7 times of 3-mercaptopropyltrimethoxysilane by mass of a solid phase material, reacting for 1-3h while stirring, and drying in an oven at 80 ℃ to obtain the product.
The invention has the beneficial effects that:
(1) the surface of the graphene oxide has rich oxygen-containing groups such as hydroxyl groups and carboxyl groups, so that the graphene oxide has a certain adsorption effect on heavy metal ions, meanwhile, the gel form of the graphene oxide with a two-dimensional surface layer structure has a porous net structure, so that the ion diffusion can be improved, the mass transfer resistance can be reduced, the characteristics of high adsorption rate, large adsorption capacity and the like are shown, the heavy metal ions can form microcrystalline minerals on the surface of the basic iron oxide, and the adsorption efficiency is improved, and the adsorption selectivity and stability are also improved by compounding the basic iron oxide.
(2) Polypyrrole is a common conductive compound, has the advantages of easy preparation, no toxicity, no harm, environmental stability, autoxidation reducibility and the like, is mostly used for preparing composite electrodes, and is used for recovering heavy metals through process reduction.
(3) The sulfhydryl group can be chelated with heavy metal ions in a covalent bond or coordination bond form to form a spatial reticular chelate with low solubility, so that the immobilization effect is further improved, and the bioavailability of the heavy metal is reduced.
(4) The technical scheme provided by the application also comprises a soil conditioner, and the soil ecological environment can be improved while the heavy metal is fixed and the bioavailability of the heavy metal is reduced, so that the effects of synchronously repairing and improving the polluted soil are achieved.
Detailed Description
The invention is further described with reference to the following examples.
Example 1
A heavy metal soil remediation agent comprises a heavy metal adsorption fixing agent and a soil conditioning agent, and the mass ratio of the heavy metal adsorption fixing agent to the soil conditioning agent is 10: 6, the heavy metal adsorption fixing agent consists of 100 parts of basic iron oxide-graphene oxide gel powder and 37 parts of sulfydryl modified iron oxide-polypyrrole composite particles;
the soil conditioner comprises a loosening agent, a mineral source conditioner and a water-retaining agent, and the mass percentage of the soil conditioner is 3: 5: 2;
the bulking agent is talcum powder, the mineral source conditioner is bentonite, and the water-retaining agent is chitosan and polyvinyl alcohol;
the preparation method of the alkali type iron oxide-graphene oxide gel powder comprises the following steps:
(a) preparation of basic iron oxide
Preparing basic iron oxide by solid-phase method and using FeCl3·6H2Ball milling with O as iron source and urea as hydroxyl source in ball mill3·6H2The molar ratio of O to urea is 1:4-6, the ball milling time is 1-3h, after the ball milling is finished, the product is aged for 12-24h in a water bath at 50-70 ℃, and then the product is washed by distilled water and freeze-dried to prepare basic ferric oxide;
(b) preparation of gel powder
Ultrasonically dispersing graphene oxide in distilled water, wherein the solid-liquid ratio is 1 g: 1L, adding 20wt.% of hydrazine hydrate solution accounting for 20-30% of the volume of the system, adding 0.8-1 times of basic iron oxide in mass of solid phase material, uniformly mixing, transferring to a hydrothermal reaction kettle, carrying out hydrothermal temperature of 200 ℃ and 220 ℃, reacting for 6-10h, soaking with distilled water after the reaction is finished and cooled, changing water every 12h until the solution is neutral to obtain hydrogel, and freeze-drying, drying and crushing;
the preparation method of the sulfydryl modified iron oxide-polypyrrole composite particle comprises the following steps: nano Fe2O3Ultrasonically dispersing in distilled water, wherein the solid-liquid ratio is 2 g: 1L, adding polyvinylpyrrolidone with the mass of 0.2-0.3 times of that of a solid phase material, mechanically stirring, adding pyrrole with the volume of 0.05% of the system volume, continuously stirring, dropwise adding 4.0g/L ferric chloride solution with the volume of 20-30% of the system volume, continuously stirring for 5h, centrifuging, washing with deionized water and ethanol respectively, and mixing the product according to the material-liquid ratio of 1: 5-20, adding ethanol, magnetically stirring in a water bath at a constant temperature of 50 ℃, adding 0.5-0.7 times of 3-mercaptopropyltrimethoxysilane by mass of a solid phase material, reacting for 1-3h while stirring, and drying in an oven at 80 ℃ to obtain the product.
Example 2
A heavy metal soil remediation agent comprises a heavy metal adsorption fixing agent and a soil conditioning agent, and the mass ratio of the heavy metal adsorption fixing agent to the soil conditioning agent is 10: 6, the heavy metal adsorption fixing agent consists of 100 parts of basic iron oxide-graphene oxide gel powder and 37 parts of iron oxide-polypyrrole composite particles;
the soil conditioner comprises a loosening agent, a mineral source conditioner and a water-retaining agent, and the mass percentage of the soil conditioner is 3: 5: 2;
the bulking agent is talcum powder, the mineral source conditioner is bentonite, and the water-retaining agent is chitosan and polyvinyl alcohol;
the preparation method of the alkali type iron oxide-graphene oxide gel powder comprises the following steps:
(a) preparation of basic iron oxide
Preparing basic iron oxide by solid-phase method and using FeCl3·6H2Ball milling with O as iron source and urea as hydroxyl source in ball mill3·6H2The molar ratio of O to urea is 1:4-6, the ball milling time is 1-3h, after the ball milling is finished, the product is aged for 12-24h in a water bath at 50-70 ℃, and then the product is washed by distilled water and freeze-dried to prepare basic ferric oxide;
(b) preparation of gel powder
Ultrasonically dispersing graphene oxide in distilled water, wherein the solid-liquid ratio is 1 g: 1L, adding 20wt.% of hydrazine hydrate solution accounting for 20-30% of the volume of the system, adding 0.8-1 times of basic iron oxide in mass of solid phase material, uniformly mixing, transferring to a hydrothermal reaction kettle, carrying out hydrothermal temperature of 200 ℃ and 220 ℃, reacting for 6-10h, soaking with distilled water after the reaction is finished and cooled, changing water every 12h until the solution is neutral to obtain hydrogel, and freeze-drying, drying and crushing;
the preparation method of the iron oxide-polypyrrole composite particles comprises the following steps: nano Fe2O3Ultrasonically dispersing in distilled water, wherein the solid-liquid ratio is 2 g: 1L, adding polyvinylpyrrolidone with the mass of 0.2-0.3 times of that of a solid phase material, mechanically stirring, adding pyrrole with the volume of 0.05% of the system volume, continuously stirring, dropwise adding 4.0g/L ferric chloride solution with the volume of 20-30% of the system volume, continuously stirring for 5h, centrifuging, washing with deionized water and ethanol respectively, and drying in an oven at 80 ℃.
Example 3
A heavy metal soil remediation agent comprises a heavy metal adsorption fixing agent and a soil conditioning agent, and the mass ratio of the heavy metal adsorption fixing agent to the soil conditioning agent is 10: 2, the heavy metal adsorption fixing agent consists of 100 parts of basic iron oxide-graphene oxide gel powder and 88 parts of sulfydryl modified iron oxide-polypyrrole composite particles;
the soil conditioner comprises a loosening agent, a mineral source conditioner and a water-retaining agent, and the mass percentage of the soil conditioner is 3: 5: 2;
the bulking agent is talcum powder, the mineral source conditioner is bentonite, and the water-retaining agent is chitosan and polyvinyl alcohol;
the preparation method of the alkali type iron oxide-graphene oxide gel powder comprises the following steps:
(a) preparation of basic iron oxide
Preparing basic iron oxide by solid-phase method and using FeCl3·6H2Ball milling with O as iron source and urea as hydroxyl source in ball mill3·6H2The molar ratio of O to urea is 1:4-6, the ball milling time is 1-3h, after the ball milling is finished, the product is aged for 12-24h in a water bath at 50-70 ℃, and then the product is washed by distilled water and freeze-dried to prepare basic ferric oxide;
(b) preparation of gel powder
Ultrasonically dispersing graphene oxide in distilled water, wherein the solid-liquid ratio is 1 g: 1L, adding 20wt.% of hydrazine hydrate solution accounting for 20-30% of the volume of the system, adding 0.8-1 times of basic iron oxide in mass of solid phase material, uniformly mixing, transferring to a hydrothermal reaction kettle, carrying out hydrothermal temperature of 200 ℃ and 220 ℃, reacting for 6-10h, soaking with distilled water after the reaction is finished and cooled, changing water every 12h until the solution is neutral to obtain hydrogel, and freeze-drying, drying and crushing;
the preparation method of the sulfydryl modified iron oxide-polypyrrole composite particle comprises the following steps: nano Fe2O3Ultrasonically dispersing in distilled water, wherein the solid-liquid ratio is 2 g: 1L, adding polyvinylpyrrolidone with the mass of 0.2-0.3 times of that of a solid phase material, mechanically stirring, adding pyrrole with the volume of 0.05% of the system volume, continuously stirring, dropwise adding 4.0g/L ferric chloride solution with the volume of 20-30% of the system volume, continuously stirring for 5h, centrifuging, washing with deionized water and ethanol respectively, and mixing the product according to the material-liquid ratio of 1: 5-20, adding ethanol, magnetically stirring in a water bath at a constant temperature of 50 ℃, adding 0.5-0.7 times of 3-mercaptopropyltrimethoxysilane by mass of a solid phase material, reacting for 1-3h while stirring, and drying in an oven at 80 ℃ to obtain the product.
Example 4
A heavy metal soil remediation agent comprises a heavy metal adsorption fixing agent and a soil conditioning agent, and the mass ratio of the heavy metal adsorption fixing agent to the soil conditioning agent is 10: 6, the heavy metal adsorption fixing agent consists of 100 parts of basic iron oxide-graphene oxide gel powder and 37 parts of sulfydryl modified iron oxide-polypyrrole composite particles;
the soil conditioner comprises a pH regulator, a loosening agent, a mineral source conditioner and a water-retaining agent, and the mass percentage of the soil conditioner is 2: 3: 5: 2;
the pH regulator is calcium carbonate, the bulking agent is apatite, the mineral source conditioner is diatomite and sepiolite, and the water-retaining agent is chitosan and polyethylene glycol;
the preparation method of the alkali type iron oxide-graphene oxide gel powder comprises the following steps:
(a) preparation of basic iron oxide
Preparing basic iron oxide by solid-phase method and using FeCl3·6H2Ball milling with O as iron source and urea as hydroxyl source in ball mill3·6H2The molar ratio of O to urea is 1:4-6, the ball milling time is 1-3h, after the ball milling is finished, the product is aged for 12-24h in a water bath at 50-70 ℃, and then the product is washed by distilled water and freeze-dried to prepare basic ferric oxide;
(b) preparation of gel powder
Ultrasonically dispersing graphene oxide in distilled water, wherein the solid-liquid ratio is 1 g: 1L, adding 20wt.% of hydrazine hydrate solution accounting for 20-30% of the volume of the system, adding 0.8-1 times of basic iron oxide in mass of solid phase material, uniformly mixing, transferring to a hydrothermal reaction kettle, carrying out hydrothermal temperature of 200 ℃ and 220 ℃, reacting for 6-10h, soaking with distilled water after the reaction is finished and cooled, changing water every 12h until the solution is neutral to obtain hydrogel, and freeze-drying, drying and crushing;
the preparation method of the sulfydryl modified iron oxide-polypyrrole composite particle comprises the following steps: nano Fe2O3Ultrasonically dispersing in distilled water, wherein the solid-liquid ratio is 2 g: 1L, adding polyvinylpyrrolidone with the mass of 0.2-0.3 times of that of a solid phase material, mechanically stirring, adding pyrrole with the volume of 0.05% of the system volume, continuously stirring, dropwise adding 4.0g/L ferric chloride solution with the volume of 20-30% of the system volume, continuously stirring for 5h, centrifuging, washing with deionized water and ethanol respectively, and mixing the product according to the material-liquid ratio of 1: adding ethanol 5-20, magnetic stirring in water bath at 50 deg.C, adding 05-0.7 times of solid phase material mass of 3-mercaptopropyltrimethoxysilane, stirring and reacting for 1-3h, and drying in an oven at 80 ℃.
Comparative example
A soil conditioner consisting of talcum powder, bentonite, chitosan and polyvinyl alcohol, which comprises the following components in percentage by mass: 5: 2.
examples of the experiments
The heavy metal soil remediation agent is uniformly applied to the polluted soil, ploughing and mixing are carried out, stacking and aging are carried out for 10-30d, turning is carried out once every 3-5 days, the heavy metal soil remediation agent is applied according to the using amount of 200 kg/mu, the contents of Cr, Cd, Hg and Pb in the soil before and after the heavy metal soil remediation agent in the examples 1-4 and the regulator in the comparative example (the using amount of the comparative example is 75 kg/mu) are applied are measured by a leaching method, and the measurement results are shown in Table 1.
The rice is planted in the soil before the application of the repairing agent as a control, the rice is also planted in the soil after the application, the heavy metal content in the rice is measured, and the measurement result is shown in table 2.
TABLE 1 heavy metal content in soil before and after application
Before application | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example | |
Cr(mg/kg) | 65.8 | 18.7 | 22.5 | 20.2 | 19.8 | 62.7 |
Cd(mg/kg) | 0.46 | 0.19 | 0.23 | 0.22 | 0.20 | 0.43 |
Hg(mg/kg) | 0.52 | 0.13 | 0.16 | 0.15 | 0.13 | 0.45 |
Pb(mg/kg) | 74.7 | 25.9 | 28.4 | 26.2 | 25.5 | 66.4 |
TABLE 2 content of heavy metals in rice before and after application
Before application | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example | |
Cr(mg/kg) | 0.263 | 0.117 | 0.149 | 0.136 | 0.113 | 0.237 |
Cd(mg/kg) | 0.186 | 0.089 | 0.112 | 0.099 | 0.091 | 0.195 |
Hg(mg/kg) | 0.038 | 0.004 | 0.015 | 0.012 | 0.006 | 0.039 |
Pb(mg/kg) | 0.125 | 0.067 | 0.074 | 0.073 | 0.066 | 0.123 |
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (6)
1. The heavy metal soil remediation agent is characterized by comprising a heavy metal adsorption fixing agent and a soil conditioning agent, and the mass fraction ratio of the heavy metal adsorption fixing agent to the soil conditioning agent is 10: 1-10, wherein the heavy metal adsorption fixing agent consists of basic iron oxide-graphene oxide gel powder and iron oxide-polypyrrole composite particles, the relative mass ratio of the basic iron oxide-graphene oxide gel powder to the iron oxide-polypyrrole composite particles is 100:1-100, the iron oxide-polypyrrole composite particles are sulfydryl modified iron oxide-polypyrrole composite particles, and the soil conditioner is one or more of a pH regulator, a loosening agent, a mineral source conditioner and a water-retaining agent;
the preparation method of the alkali type iron oxide-graphene oxide gel powder comprises the following steps:
(a) preparation of basic iron oxide
Preparing basic iron oxide by a solid phase methodFeCl3·6H2Ball milling with O as iron source and urea as hydroxyl source in ball mill3·6H2The molar ratio of O to urea is 1:4-6, the ball milling time is 1-3h, after the ball milling is finished, the product is aged for 12-24h in a water bath at 50-70 ℃, and then the product is washed by distilled water and freeze-dried to prepare basic ferric oxide;
(b) preparation of gel powder
Ultrasonically dispersing graphene oxide in distilled water, wherein the solid-liquid ratio is 1 g: 1L, adding 20wt.% of hydrazine hydrate solution accounting for 20-30% of the volume of the system, adding 0.8-1 times of basic iron oxide in mass of solid phase material, uniformly mixing, transferring to a hydrothermal reaction kettle, carrying out hydrothermal temperature of 200 ℃ and 220 ℃, reacting for 6-10h, soaking with distilled water after the reaction is finished and cooled, changing water every 12h until the solution is neutral to obtain hydrogel, and freeze-drying, drying and crushing;
the preparation method of the sulfydryl modified iron oxide-polypyrrole composite particle comprises the following steps: nano Fe2O3Ultrasonically dispersing in distilled water, wherein the solid-liquid ratio is 2 g: 1L, adding polyvinylpyrrolidone with the mass of 0.2-0.3 times of that of a solid phase material, mechanically stirring, adding pyrrole with the volume of 0.05% of the system volume, continuously stirring, dropwise adding 4.0g/L ferric chloride solution with the volume of 20-30% of the system volume, continuously stirring for 5h, centrifuging, washing with deionized water and ethanol respectively, and mixing the product according to the material-liquid ratio of 1: 5-20, adding ethanol, magnetically stirring in a water bath at a constant temperature of 50 ℃, adding 0.5-0.7 times of 3-mercaptopropyltrimethoxysilane by mass of a solid phase material, reacting for 1-3h while stirring, and drying in an oven at 80 ℃ to obtain the product.
2. The heavy metal soil remediation agent of claim 1 wherein said heavy metal adsorbing and immobilizing agent acts on one or more of Cr, Cd, Hg, Pb.
3. The heavy metal soil remediation agent of claim 1, wherein said pH-adjusting agent is one or more of calcium carbonate, calcium sulfate, magnesium hydroxide, oxalic acid, ferrous sulfate.
4. The heavy metal soil remediation agent of claim 1, wherein said bulking agent is one or more of talc, fly ash, maifanite, ground phosphate rock, apatite.
5. The heavy metal soil remediation agent of claim 1 wherein said mineral-derived conditioning agent is one or more of bentonite, diatomaceous earth, sepiolite, vermiculite.
6. The heavy metal soil remediation agent of claim 1, wherein said water retaining agent is one or more of chitosan, polyacrylic acid, polyvinyl alcohol, polyethylene glycol.
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