CN114686240A - Reducing agent for heavy metal contaminated soil and use method thereof - Google Patents
Reducing agent for heavy metal contaminated soil and use method thereof Download PDFInfo
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- CN114686240A CN114686240A CN202210314999.1A CN202210314999A CN114686240A CN 114686240 A CN114686240 A CN 114686240A CN 202210314999 A CN202210314999 A CN 202210314999A CN 114686240 A CN114686240 A CN 114686240A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K17/00—Soil-conditioning materials or soil-stabilising materials
- C09K17/40—Soil-conditioning materials or soil-stabilising materials containing mixtures of inorganic and organic compounds
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/40—Bio-organic fraction processing; Production of fertilisers from the organic fraction of waste or refuse
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Abstract
The application discloses a reducing agent for heavy metal contaminated soil and a using method thereof, wherein the reducing agent for heavy metal contaminated soil comprises organic matter compost and modified nano zero-valent iron, wherein the mass ratio of the organic matter compost to the modified nano zero-valent iron is (4-10) to (0.1-0.6); the modified nano zero-valent iron is prepared from the following components in parts by mass: iron salt: 3-5 parts; reducing agent: 3-6 parts; a stabilizer: 2-4 parts; alcoholic solution: 100-200 parts; silane coupling agent: 1-3 parts; dimercaptothreitol: 1-2 parts. The reducing agent for heavy metal contaminated soil generates harmless by-products in the using process, and the repairing effect is more prominent.
Description
Technical Field
The application relates to the field of soil pollution treatment, in particular to a reducing agent for heavy metal polluted soil and a using method thereof.
Background
The waste discharge of the traditional industries such as chromium salt production, electroplating, leather dyeing and finishing and the like contains more hexavalent chromium with high solubility and high toxicity, and the hexavalent chromium can permeate into the surrounding soil or underground water to cause ecological pollution and enter the human body along with an ecological chain to seriously threaten the health of the human body.
At present, the mature restoration method of hexavalent chromium pollution is to adopt a reducing agent to carry out chemical reduction to obtain trivalent chromium with low toxicity. Commonly used reducing agents include sulfur-based reducing agents such as sodium dithionite, thiosulfate and polysulfide, and organic reducing agents such as molasses. However, sulfur reducing agents generate harmful gases such as hydrogen sulfide in the using process, and have potential harm to human bodies; but the repair effect of the molasses in the using process is poor.
Disclosure of Invention
In order to solve the problems of hazardous byproducts generated in the repairing process and poor repairing effect, the application provides a reducing agent for heavy metal contaminated soil and a using method thereof.
In a first aspect, the application provides a reducing agent for heavy metal contaminated soil, which comprises organic compost and modified nano zero-valent iron in a mass ratio of (4-10) to (0.1-0.6); the modified nano zero-valent iron is prepared from the following components in parts by mass:
iron salt: 3-5 parts;
reducing agent: 3-6 parts;
a stabilizer: 2-4 parts;
alcoholic solution: 100-200 parts;
silane coupling agent: 1-3 parts;
dimercaptothreitol: 1-2 parts.
By adopting the technical scheme, the organic matter compost contains a large amount of humic acid, fulvic acid and other components, and active groups such as aldehyde groups, phenol groups, quinone groups and the like contained in the humic acid and the fulvic acid can reduce hexavalent chromium ions with high solubility, strong oxidizability and high toxicity into trivalent chromium ions with low solubility and low toxicity. The modified nano zero-valent iron has excellent adsorbability and reducibility due to the specific nano effect, and can efficiently and quickly realize the reduction of hexavalent chromium.
In addition, in the re-preparation process of the modified nano zero-valent iron, the agglomeration phenomenon can be reduced on one hand through the compound modification of the silane coupling agent and the dimercaptothreitol; on the other hand, dimercaptothreitol with extremely strong reducibility can be adsorbed on the surface of the nano zero-valent iron, so that the reduction and remediation effects on soil are further improved.
Preferably, the modified nanoscale zero-valent iron is prepared by the following method:
s101: dissolving ferric salt into an alcohol solution, adding a stabilizer, and uniformly mixing to obtain a pre-reaction solution;
s102: adding a reducing agent into the pre-reaction solution, continuously mixing to obtain a nano zero-valent iron solution, and separating and drying to obtain nano zero-valent iron;
s103: adding the nano zero-valent iron into water, sequentially adding a silane coupling agent and dimercaptothreitol, uniformly mixing, separating and drying to obtain the modified nano zero-valent iron.
By adopting the technical scheme, firstly, the stabilizing agent is added into the iron ion solution, so that the agglomeration tendency of the reduced nano zero-valent iron can be effectively inhibited, and the uniformity and stability of the grain size of the nano zero-valent iron can be guaranteed. Secondly, adding a silane coupling agent and dimercaptothreitol, wherein the silane coupling agent generates a silanol group after hydrolysis, so that the silanol group is adsorbed on the surface of the nano zero-valent iron and is mutually crosslinked to form a net structure, and the dimercaptothreitol can be coupled with the silane coupling agent through an active group, so that the dimercaptothreitol is adsorbed on the surface of the nano zero-valent iron, and the reduction repair effect of the nano zero-valent iron is enhanced.
Preferably, the silane coupling agent is 3-propylmercaptotrimethylsilane.
By adopting the technical scheme, except for the coupling effect, the 3-propylmercapto-trimethyl silane molecular chain contains mercapto which can generate coordination with metal ions, so that adsorption effect is generated on reduced trivalent chromium ions, the balance of hexavalent chromium reduction reaction is changed, and the reduction reaction is promoted to be carried out.
Preferably, the stabilizer is one or more of diethylene glycol, triethylene glycol, polyethylene glycol and polyvinylpyrrolidone.
By adopting the technical scheme, the stabilizing agent can effectively promote the dispersion of the nano zero-valent iron and ensure the nano effect of the nano zero-valent iron.
Preferably, tannic acid is further added in step S103, and the tannic acid is added together with the silane coupling agent.
By adopting the technical scheme, the tannin molecules contain ortho-phenolic hydroxyl, can perform a complex reaction with ions on the surface of the nano zero-valent iron, and is cooperatively matched with the reticular silane membrane, so that more active sites are provided for the attachment of dimercaptothreitol, and the reduction repair effect of the modified nano zero-valent iron is enhanced. Meanwhile, the tannic acid can be coordinated with trivalent chromium ions, so that the balance of hexavalent chromium reaction is changed, and the reduction of hexavalent chromium is promoted.
Preferably, the organic compost is prepared according to the following method:
mixing organic waste and humus according to the mass ratio of (2-4) to 1, and fermenting at the temperature of 40-60 ℃ and the humidity of 50-60%, wherein the compost fermentation time is 3-4 weeks.
By adopting the technical scheme, organic matter compost with a large amount of humic acid and fulvic acid is obtained through full fermentation, so that a superior hexavalent chromium reduction remediation effect is obtained. The organic waste is not required to be specially treated, and generally crop straws, plant stems and leaves, livestock manure, wood chips and the like are adopted.
Preferably, the reducing agent for heavy metal contaminated soil also comprises sodium polyacrylate as a raw material, and the mass ratio of the sodium polyacrylate to the modified nano zero-valent iron is (0.3-1) to (0.1-0.6).
By adopting the technical scheme, the hexavalent chromium ions are firmly adsorbed in the soil due to the porosity and strong adsorption of the soil; meanwhile, soil particles are easy to form a flocculation structure, so that a large amount of water is coated, and the flowing and reduction of hexavalent chromium ions are inhibited. This application utilizes its infiltration and dispersion to soil particles through adopting sodium polyacrylate, can effectual release moisture, promotes the flow of soil particles and hexavalent chromium ion, improves the reduction effect.
In a second aspect, the application provides a use method of the reducing agent for the heavy metal contaminated soil, which comprises the following steps:
s201: adding organic matter compost accounting for 4-10% of the weight of the soil into the hexachromium polluted soil, adding water until the water content is 40-50%, and stirring into slurry to obtain rough-treated soil;
s202: and adding the modified nano zero-valent iron nano into the roughly treated soil, uniformly mixing, and maintaining for 20-30 days.
By adopting the technical scheme, under the synergistic effect of the organic matter compost and the modified nano zero-valent iron sodium, the remediation effect on chromium-polluted soil can be effectively improved, and harmful substances harmful to human bodies are not easily generated.
Preferably, sodium polyacrylate is also added in the step S201, and the mass ratio of the sodium polyacrylate to the modified nano zero-valent iron is (0.3-1): 0.1-0.6.
By adopting the technical scheme, the contact probability of hexavalent chromium ions, humic acid and modified nano zero-valent iron in the soil is improved by utilizing the sodium polyacrylate, and the improvement of the soil reduction remediation effect is effectively promoted.
In summary, the present application has the following beneficial effects:
1. in the application, the modified nano zero-valent iron with the surface adsorbed with dimercaptothreitol is matched with organic matter compost, so that the reduction remediation effect on the hexavalent chromium polluted soil is obviously improved.
2. In the application, the nano zero-valent iron is pre-modified by adopting 3-propylmercaptotrimethylsilane, so that a molecular chain containing sulfydryl is obtained by in-situ polymerization on the surface of the nano zero-valent iron, and the sulfydryl and trivalent chromium ions are subjected to a complex reaction, so that the reduction of the hexachromic ions is facilitated, and the soil remediation effect is improved.
3. In the application, by adopting the sodium polyacrylate, the mobility of soil particles and hexavalent chromium ions is effectively promoted, the contact probability of hexavalent chromium and a reducing agent is improved, and the repair effect is improved.
Detailed Description
Preparation example of modified Nano zero-valent iron
Preparation example 1, a modified nano zero-valent iron was prepared as follows:
s101: taking 20g FeCl2·4H2Adding O into 4L butanediol solution, stirring for 20min to allow FeCl2·4H2Dissolving O, adding 16g of diglycol (a stabilizing agent), and continuously stirring for 10min to obtain a pre-reaction solution;
s102: adding 24g of sodium borohydride (reducing agent) into the pre-reaction solution, and stirring for 1h to obtain a black nano zero-valent iron solution; separating out particles by a magnetic separation method and drying to obtain the nano zero-valent iron;
s103: and (2) adding the nano zero-valent iron obtained in the step (S102) into 1L of purified water, sequentially adding 8g of tannic acid, 10g of 3-propylmercaptotrimethylsilane (silane coupling agent) and 8g of dimercaptothreitol, stirring for 30min, separating particles by using a magnetic separation method, and drying to obtain the modified nano zero-valent iron.
Preparation example 2, a modified nano zero-valent iron was prepared as follows:
s101: taking 12g FeCl2·4H2Adding O into 1.2L of glycol solution, and stirring for 20min to allow FeCl2·4H2Dissolving O, adding 8g of polyethylene glycol (stabilizer), and continuously stirring for 10min to obtain a pre-reaction solution;
s102: adding 16g of sodium borohydride (reducing agent) into the pre-reaction solution, and stirring for 1h to obtain a black nano zero-valent iron solution; separating out particles by a magnetic separation method and drying to obtain nano zero-valent iron;
s103: and (3) adding the nano zero-valent iron obtained in the step (S102) into 1L of purified water, sequentially adding 4g of tannic acid, 4g of 3-propylmercaptotrimethylsilane (silane coupling agent) and 4g of dimercaptothreitol, stirring for 30min, separating particles by using a magnetic separation method, and drying to obtain the modified nano zero-valent iron.
Preparation example 3, a modified nano zero-valent iron, differs from preparation example 1 in that in step S103, the silane coupling agent used is γ -aminopropyltriethoxysilane.
Preparation example 4, a modified nano zero-valent iron, differs from preparation example 1 in that, in step S103, polyvinylpyrrolidone is used as a stabilizer.
Preparation example 5, a modified nano zero-valent iron, was different from preparation example 1 in that tannic acid was not added in step S103.
Preparation example 6, a modified nano zero-valent iron, differs from preparation example 1 in that tannic acid and a silane coupling agent are not added in step S103.
Preparation example 7, a modified nano zero-valent iron, differs from preparation example 1 in that dimercaptothreitol is not added in step S103.
Organic matter compost preparation example
Preparation example a, an organic compost was prepared as follows:
mixing 100 kg of corn straw scraps, cow dung, leaves, sawdust (organic plant waste) and 25 kg of humus soil, stirring uniformly, fermenting at 50 +/-5 ℃ and relative humidity of 55 +/-5%, and performing intermittent ventilation and oxygen supply with air flow of 0.2m3Ventilating every 8 hours for 20 min; turning over the piles once every day, and fermenting for 3 weeks to obtain the organic compost.
Preparation example b, an organic compost was prepared as follows:
mixing 100 kg of rice straw scraps, waste vegetable leaves, pig manure (organic plant waste) and 50 kg of humus soil, uniformly stirring, and fermenting at the temperature of 45 +/-5 ℃ and the relative humidity of 55 +/-5%; adopts intermittent ventilation and oxygen supply, and the air flow is 0.1m3Ventilating every 8 hours for 30 min; turning over the piles once every day, and fermenting for 4 weeks to obtain the organic compost.
Examples
Example 1, a method for using a reducing agent for heavy metal contaminated soil, comprising the following operations:
s201: adding 4 kg of organic matter compost (prepared in preparation example a) to 100 kg of six-chromium-polluted soil, adding water to reach the water content of 40%, adding 0.3 kg of sodium polyacrylate, and stirring into a slurry state to obtain crude treated soil;
s202: and adding 0.1 kg of modified nano zero-valent iron nano (prepared in preparation example 1) into the roughly treated soil, uniformly mixing, and maintaining for 20 days.
Wherein, the molecular weight of the sodium polyacenoate adopted in the step S201 is less than 10000.
Embodiment 2, a method for using a reducing agent for heavy metal contaminated soil, comprising the following operations:
s201: adding 10 kg of organic matter composts (prepared in preparation example a) to 100 kg of six-chromium-polluted soil, adding water to reach the water content of 50%, adding 1 kg of sodium polyacrylate, and stirring into a slurry state to obtain crude treated soil;
s202: and adding 0.6 kg of modified nano zero-valent iron nano (prepared in preparation example 1) into the roughly treated soil, uniformly mixing, and maintaining for 30 days.
Wherein, the molecular weight of the sodium polyacenoate adopted in the step S201 is less than 10000.
Example 3, a method for using a reducing agent for heavy metal contaminated soil, is different from example 1 in that the reducing agent prepared in preparation example b is used in step S201.
Example 4, a method for using a reducing agent for heavy metal contaminated soil, which is different from example 1, is that in step S202, the modified nano zero-valent iron nano prepared in preparation example 2 is used.
Example 5, a method for using a reducing agent for heavy metal contaminated soil, which is different from example 1 in that the modified nano zero-valent iron nano prepared in preparation example 3 is used in step S202.
Example 6, a method for using a reducing agent for heavy metal contaminated soil, which is different from example 1, is that in step S202, the modified nano zero-valent iron nano prepared in preparation example 4 is used.
Example 7, a method for using a reducing agent for heavy metal contaminated soil, which is different from example 1 in that the modified nano zero-valent iron nano prepared in preparation example 5 is used in step S202.
Example 8, a method for using a reducing agent for heavy metal contaminated soil, is different from example 1 in that sodium polyacrylate is not added in step S201.
Comparative example
Comparative example 1, a method for using a reducing agent for heavy metal contaminated soil, is different from example 1 in that the modified nano zero-valent iron nano prepared in preparation example 6 is used in step S202.
Comparative example 2, a method for using a reducing agent for heavy metal contaminated soil, is different from example 1 in that the modified nano zero-valent iron nano prepared in preparation example 7 is used in step S202.
Comparative example 3, a method for using a reducing agent for heavy metal contaminated soil, is different from example 1 in that, in step S202, the modified nano zero-valent iron nano prepared in preparation example 1 is replaced with an equal amount of commercially available nano zero-valent iron (20 nm).
Comparative example 4, a method for using a reducing agent for heavy metal contaminated soil, comprising the following operations:
s201: adding water to 100 kilograms of six-chromium-polluted soil until the water content is 50%, adding 2 kilograms of sodium polyacrylate, and stirring into a slurry state to obtain crude treated soil;
s202: and adding 6 kg of modified nano zerovalent iron nano (prepared in preparation example 1) into the roughly treated soil, uniformly mixing, and maintaining for 30 days.
Performance test
The soil remediation effect test method comprises the following steps: maintenance and remediation were performed on the soil contaminated with chromium according to the operations in the above examples and comparative examples, and the contents of six chromium (mg/kg) in the soil before and after remediation were measured and the reduction rate (%) of the hexavalent chromium content thereof was calculated.
TABLE 1 soil remediation Effect test results
And (3) analyzing test results:
(1) by combining examples 1-8 and comparative examples 1-3 and combining table 1, it can be seen that compared with comparative examples 1-3, the reduction repair effect of hexavalent chromium in soil is remarkably improved by adopting the nano zero-valent iron modified by the silane coupling agent and the dimercaptothreitol in examples 1-8. The reason may be that, firstly, the nano zero-valent iron has a large specific surface area and a large reduction activity, so that hexavalent chromium ions can be effectively reduced into trivalent chromium ions, and a repairing effect is achieved. Silane coupling agent and dimercapto threitol are adopted for modification, wherein the silane coupling agent can be attached to the surface of the nano zero-valent iron to form a reticular silane film, and the adsorption of the dimercapto threitol is promoted. Because dimercaptothreitol has good reducibility, and is attached to the surface of the nano zero-valent iron, the reduction repair effect of dimercaptothreitol can be further improved.
Meanwhile, the sulfydryl contained on the surface of the nano zero-valent iron can coordinate with trivalent chromium, so that the balance of the hexavalent chromium reduction reaction is promoted to move rightwards. In addition. The reticular silane film can also inhibit the agglomeration trend of the nano zero-valent iron and ensure the dispersibility of the nano zero-valent iron.
(2) By combining the examples 1 to 8 and the comparative example 4 and combining the table 1, compared with the comparative example 4, the organic compost is added in the examples 1 to 8, so that the restoration effect on the hexavalent chromium soil is effectively improved. The reason for this is that the organic compost contains a large amount of humic acid, fulvic acid and other components, and active groups such as aldehyde group, phenol group, quinone group and the like contained in the humic acid and fulvic acid can reduce hexavalent chromium ions having high solubility, strong oxidizability and high toxicity into trivalent chromium ions having low solubility and low toxicity.
(3) By combining the examples 1 and 5 and the table 1, it can be seen that the addition of a proper amount of tannic acid during the modification of the nano zero-valent iron is helpful to improve the repairing effect of the obtained modified nano zero-valent iron. The reason may be that tannic acid can form a complex membrane with ions on the surface of the nano zero-valent iron, so that more active sites are provided for the attachment of dimercaptothreitol; on the other hand, the tannic acid can coordinate with trivalent chromium ions, so that the balance of hexavalent chromium reaction is changed, and the reduction of hexavalent chromium is promoted.
(4) By combining example 1 and example 8 and table 1, it can be seen that the effect of improving the remediation effect of hexavalent chromium soil can also be improved by adding sodium polyacrylate in example 1, compared with example 8. The reason for this is probably that sodium polyacrylate has a better dispersing effect on soil particles, can effectively destroy the flocculation structure in soil, and promotes the flow of water, thereby improving the contact probability of hexavalent chromium with humic acid and modified nano zero-valent iron, and promoting the reduction of hexavalent chromium.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (9)
1. The reducing agent for heavy metal contaminated soil is characterized by comprising organic matter compost and modified nano zero-valent iron in a mass ratio of (4-10) to (0.1-0.6); the modified nano zero-valent iron is prepared from the following components in parts by mass:
iron salt: 3-5 parts;
reducing agent: 3-6 parts;
a stabilizer: 2-4 parts;
alcoholic solution: 100-200 parts;
silane coupling agent: 1-3 parts;
dimercaptothreitol: 1-2 parts.
2. The reducing agent for heavy metal contaminated soil according to claim 1, wherein the modified nanoscale zero-valent iron is prepared by the following method:
s101: dissolving ferric salt into an alcohol solution, adding a stabilizer, and uniformly mixing to obtain a pre-reaction solution;
s102: adding a reducing agent into the pre-reaction solution, continuously mixing to obtain a nano zero-valent iron solution, and separating and drying to obtain nano zero-valent iron;
s103: adding the nano zero-valent iron into water, sequentially adding a silane coupling agent and dimercaptothreitol, uniformly mixing, separating and drying to obtain the modified nano zero-valent iron.
3. The reducing agent for heavy metal contaminated soil according to claim 1, wherein 3-propylmercaptotrimethylsilane is used as the silane coupling agent.
4. The reducing agent for heavy metal contaminated soil according to claim 1, wherein the stabilizer is one or more of diethylene glycol, triethylene glycol, polyethylene glycol and polyvinylpyrrolidone.
5. The reducing agent for heavy metal contaminated soil according to claim 1, wherein 1 to 2 parts by mass of tannic acid is further added in step S103, and the tannic acid is added together with a silane coupling agent.
6. The reducing agent for heavy metal contaminated soil according to claim 1, wherein the organic compost is prepared by the following method:
mixing organic waste and humus according to the mass ratio of (2-4) to 1, and fermenting at the temperature of 40-60 ℃ and the humidity of 50-60%, wherein the compost fermentation time is 3-4 weeks.
7. The reducing agent for heavy metal contaminated soil as claimed in claim 1, wherein the reducing agent for heavy metal contaminated soil further comprises sodium polyacrylate, and the mass ratio of the sodium polyacrylate to the modified nano zero-valent iron is (0.3-1): (0.1-0.6).
8. The use method of the reducing agent for heavy metal contaminated soil according to any one of claims 1 to 7, characterized by comprising the following steps:
s201: adding organic matter compost accounting for 4-10% of the weight of the soil into the hexachromium polluted soil, adding water until the water content is 40-50%, and stirring into slurry to obtain rough-treated soil;
s202: adding the modified nano zero-valent iron nano into the roughly treated soil, uniformly mixing, and maintaining for 20-30 d.
9. The use method of the reducing agent for heavy metal contaminated soil according to claim 8, wherein sodium polyacrylate is further added in the step S201, and the mass ratio of the sodium polyacrylate to the modified nano zero-valent iron is (0.3-1): 0.1-0.6.
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| CN115895672A (en) * | 2022-11-02 | 2023-04-04 | 方文琛 | Heavy metal soil treatment method |
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